# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-ESRF-0p00GPa
_database_code_depnum_ccdc_archive 'CCDC 2427930'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-ESRF-0p00GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.445 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.9154(7)
_cell_length_b                   15.3295(11)
_cell_length_c                   11.1833(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.336(8)
_cell_angle_gamma                90
_cell_volume                     1466.69(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    651
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.4500
_cell_measurement_theta_min      2.1180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.445
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3259
_diffrn_reflns_point_group_measured_fraction_full 0.445
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.799
_diffrn_reflns_theta_min         1.981
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.445
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295375000
_diffrn_orient_matrix_UB_12      0.0144970000
_diffrn_orient_matrix_UB_13      -0.0141872000
_diffrn_orient_matrix_UB_21      -0.0300130000
_diffrn_orient_matrix_UB_22      -0.0025189000
_diffrn_orient_matrix_UB_23      -0.0350551000
_diffrn_orient_matrix_UB_31      -0.0227204000
_diffrn_orient_matrix_UB_32      0.0222768000
_diffrn_orient_matrix_UB_33      0.0052639000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1493
_reflns_number_total             1953
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1953
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0938P)²+2.3591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1785
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C11(H11), C14(H14), C12(H12), C7(H7), C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48217(8) 0.46637(4) 0.64358(6) 0.0464(3) Uani 1 1 d D U . . .
Br1 Br 1.32033(12) 0.55815(7) 0.94394(10) 0.0652(4) Uani 1 1 d D U . . .
O3 O 0.2907(8) 0.5421(4) 0.5797(5) 0.0509(19) Uani 1 1 d D U . . .
N1 N 0.6124(9) 0.5769(4) 0.7181(6) 0.0463(15) Uani 1 1 d D U . . .
O2 O 0.2927(12) 0.3093(5) 0.5307(8) 0.083(3) Uani 1 1 d D U . . .
C8 C 0.3925(11) 0.6812(6) 0.6697(8) 0.0556(14) Uani 1 1 d D U . . .
O1 O 0.7309(12) 0.3369(6) 0.7473(10) 0.096(4) Uani 1 1 d D U . . .
C9 C 0.5504(11) 0.6529(5) 0.7211(8) 0.046(2) Uani 1 1 d D U . . .
H9 H 0.619076 0.695666 0.763210 0.056 Uiso 1 1 calc R U . . .
C3 C 0.2733(11) 0.6242(6) 0.5983(8) 0.0554(14) Uani 1 1 d D U . . .
C10 C 0.7799(10) 0.5709(6) 0.7729(7) 0.0509(10) Uani 1 1 d D U . . .
C15 C 0.8701(11) 0.5293(6) 0.7097(8) 0.0511(10) Uani 1 1 d D U . . .
H15 H 0.823270 0.503422 0.633102 0.061 Uiso 1 1 calc R U . . .
C13 C 1.0997(10) 0.5641(6) 0.8758(7) 0.0514(10) Uani 1 1 d D U . . .
C11 C 0.8482(10) 0.6078(5) 0.8890(7) 0.0516(10) Uani 1 1 d D U . . .
H11 H 0.786514 0.634840 0.932803 0.062 Uiso 1 1 calc R U . . .
C14 C 1.0320(11) 0.5257(6) 0.7598(8) 0.0514(10) Uani 1 1 d D U . . .
H14 H 1.093971 0.498142 0.716744 0.062 Uiso 1 1 calc R U . . .
C12 C 1.0100(10) 0.6040(5) 0.9392(7) 0.0518(10) Uani 1 1 d D U . . .
H12 H 1.056504 0.628842 1.016646 0.062 Uiso 1 1 calc R U . . .
C7 C 0.3569(12) 0.7685(6) 0.6884(8) 0.0561(14) Uani 1 1 d D U . . .
H7 H 0.435101 0.804957 0.734858 0.067 Uiso 1 1 calc R U . . .
C4 C 0.1223(12) 0.6608(6) 0.5482(9) 0.0561(14) Uani 1 1 d D U . . .
H4 H 0.042345 0.626006 0.500205 0.067 Uiso 1 1 calc R U . . .
C2 C 0.3612(13) 0.3689(6) 0.5748(9) 0.057(3) Uani 1 1 d D U . . .
C1 C 0.6427(13) 0.3895(6) 0.7061(10) 0.062(4) Uani 1 1 d D U . . .
C5 C 0.0922(12) 0.7457(6) 0.5689(8) 0.0565(14) Uani 1 1 d D U . . .
H5 H -0.008295 0.767377 0.535333 0.068 Uiso 1 1 calc R U . . .
C6 C 0.2079(11) 0.8010(6) 0.6391(7) 0.0565(14) Uani 1 1 d D U . . .
H6 H 0.185184 0.858805 0.652451 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 2.021(6) . ?
Rh1 N1 2.090(6) . ?
Rh1 C2 1.877(8) . ?
Rh1 C1 1.835(8) . ?
Br1 C13 1.901(8) . ?
O3 C3 1.292(10) . ?
N1 C9 1.294(10) . ?
N1 C10 1.449(10) . ?
O2 C2 1.132(9) . ?
C8 C9 1.430(11) . ?
C8 C3 1.434(11) . ?
C8 C7 1.403(12) . ?
O1 C1 1.129(10) . ?
C9 H9 0.9300 . ?
C3 C4 1.420(11) . ?
C10 C15 1.368(13) . ?
C10 C11 1.390(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.395(11) . ?
C13 C14 1.398(9) . ?
C13 C12 1.354(12) . ?
C11 H11 0.9300 . ?
C11 C12 1.394(11) . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.380(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.363(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(11) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 N1 89.7(3) . . ?
C2 Rh1 O3 88.9(4) . . ?
C2 Rh1 N1 178.6(4) . . ?
C1 Rh1 O3 174.1(5) . . ?
C1 Rh1 N1 94.7(4) . . ?
C1 Rh1 C2 86.6(5) . . ?
C3 O3 Rh1 129.1(5) . . ?
C9 N1 Rh1 123.1(6) . . ?
C9 N1 C10 116.3(7) . . ?
C10 N1 Rh1 120.6(6) . . ?
C9 C8 C3 122.0(8) . . ?
C7 C8 C9 117.9(7) . . ?
C7 C8 C3 120.1(7) . . ?
N1 C9 C8 130.0(8) . . ?
N1 C9 H9 115.0 . . ?
C8 C9 H9 115.0 . . ?
O3 C3 C8 125.5(7) . . ?
O3 C3 C4 117.7(7) . . ?
C4 C3 C8 116.8(8) . . ?
C15 C10 N1 119.8(7) . . ?
C15 C10 C11 120.4(8) . . ?
C11 C10 N1 119.9(9) . . ?
C10 C15 H15 119.9 . . ?
C10 C15 C14 120.2(7) . . ?
C14 C15 H15 119.9 . . ?
C14 C13 Br1 118.6(7) . . ?
C12 C13 Br1 120.6(5) . . ?
C12 C13 C14 120.8(8) . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.4(10) . . ?
C12 C11 H11 120.3 . . ?
C15 C14 C13 118.9(10) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C13 C12 C11 120.3(7) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C8 C7 H7 119.4 . . ?
C6 C7 C8 121.2(8) . . ?
C6 C7 H7 119.4 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.4(8) . . ?
C5 C4 H4 119.3 . . ?
O2 C2 Rh1 177.2(13) . . ?
O1 C1 Rh1 173.2(13) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(8) . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 118.8(9) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 1.2(16) . . . . ?
Rh1 O3 C3 C4 -176.3(8) . . . . ?
Rh1 N1 C9 C8 -5.5(15) . . . . ?
Rh1 N1 C10 C15 48.5(12) . . . . ?
Rh1 N1 C10 C11 -131.8(7) . . . . ?
Br1 C13 C14 C15 179.6(7) . . . . ?
Br1 C13 C12 C11 -179.7(6) . . . . ?
O3 C3 C4 C5 176.6(10) . . . . ?
N1 C10 C15 C14 177.9(8) . . . . ?
N1 C10 C11 C12 -178.1(8) . . . . ?
C8 C3 C4 C5 -1.1(16) . . . . ?
C8 C7 C6 C5 -0.4(13) . . . . ?
C9 N1 C10 C15 -133.0(10) . . . . ?
C9 N1 C10 C11 46.8(12) . . . . ?
C9 C8 C3 O3 4.8(18) . . . . ?
C9 C8 C3 C4 -177.7(10) . . . . ?
C9 C8 C7 C6 178.5(9) . . . . ?
C3 C8 C9 N1 -2.2(18) . . . . ?
C3 C8 C7 C6 0.0(15) . . . . ?
C3 C4 C5 C6 0.6(16) . . . . ?
C10 N1 C9 C8 176.0(10) . . . . ?
C10 C15 C14 C13 0.8(15) . . . . ?
C10 C11 C12 C13 -0.4(11) . . . . ?
C15 C10 C11 C12 1.6(12) . . . . ?
C11 C10 C15 C14 -1.8(15) . . . . ?
C14 C13 C12 C11 -0.5(14) . . . . ?
C12 C13 C14 C15 0.3(15) . . . . ?
C7 C8 C9 N1 179.3(10) . . . . ?
C7 C8 C3 O3 -176.7(10) . . . . ?
C7 C8 C3 C4 0.8(16) . . . . ?
C4 C5 C6 C7 0.2(13) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.03617000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.377
_oxdiff_exptl_absorpt_empirical_full_min 0.470
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-04-HP-ESRF-0p97GPa
_database_code_depnum_ccdc_archive 'CCDC 2427933'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-04-HP-ESRF-0p97GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.446 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7617(4)
_cell_length_b                   14.8455(6)
_cell_length_c                   10.5564(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.550(4)
_cell_angle_gamma                90
_cell_volume                     1322.84(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1180
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.9030
_cell_measurement_theta_min      2.0260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.446
_diffrn_reflns_Laue_measured_fraction_max 0.385
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2975
_diffrn_reflns_point_group_measured_fraction_full 0.446
_diffrn_reflns_point_group_measured_fraction_max 0.385
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.796
_diffrn_reflns_theta_min         1.958
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.446
_diffrn_measured_fraction_theta_max 0.385
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284572000
_diffrn_orient_matrix_UB_12      0.0154752000
_diffrn_orient_matrix_UB_13      -0.0164023000
_diffrn_orient_matrix_UB_21      -0.0256880000
_diffrn_orient_matrix_UB_22      -0.0077360000
_diffrn_orient_matrix_UB_23      -0.0367379000
_diffrn_orient_matrix_UB_31      -0.0297459000
_diffrn_orient_matrix_UB_32      0.0214563000
_diffrn_orient_matrix_UB_33      -0.0014587000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1524
_reflns_number_total             1774
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1774
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0573P)²+1.4465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1100
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48047(6) 0.46297(3) 0.64167(4) 0.03568(18) Uani 1 1 d D U . . .
Br1 Br 1.32521(8) 0.55721(5) 0.95156(6) 0.0461(2) Uani 1 1 d D U . . .
O3 O 0.2872(6) 0.5396(3) 0.5809(4) 0.0422(12) Uani 1 1 d D U . . .
N1 N 0.6115(6) 0.5752(3) 0.7237(4) 0.0355(9) Uani 1 1 d D U . . .
O2 O 0.2926(8) 0.3044(3) 0.5169(5) 0.063(2) Uani 1 1 d D U . . .
C8 C 0.3848(8) 0.6809(4) 0.6780(5) 0.0407(8) Uani 1 1 d D U . . .
C3 C 0.2660(8) 0.6237(4) 0.6044(5) 0.0406(8) Uani 1 1 d D U . . .
C9 C 0.5469(8) 0.6539(4) 0.7311(5) 0.0399(14) Uani 1 1 d D U . . .
H9 H 0.614901 0.698130 0.776757 0.048 Uiso 1 1 calc R U . . .
O1 O 0.7295(8) 0.3282(4) 0.7448(6) 0.067(2) Uani 1 1 d D U . . .
C13 C 1.1020(7) 0.5640(4) 0.8826(5) 0.0382(6) Uani 1 1 d D U . . .
C15 C 0.8709(8) 0.5257(4) 0.7138(5) 0.0378(7) Uani 1 1 d D U . . .
H15 H 0.822530 0.496662 0.635214 0.045 Uiso 1 1 calc R U . . .
C4 C 0.1147(9) 0.6609(4) 0.5529(6) 0.0423(8) Uani 1 1 d D U . . .
H4 H 0.034508 0.625349 0.501283 0.051 Uiso 1 1 calc R U . . .
C10 C 0.7794(7) 0.5710(4) 0.7790(5) 0.0379(6) Uani 1 1 d D U . . .
C12 C 1.0145(8) 0.6091(4) 0.9497(5) 0.0391(6) Uani 1 1 d D U . . .
H12 H 1.063466 0.637258 1.028843 0.047 Uiso 1 1 calc R U . . .
C14 C 1.0363(8) 0.5221(4) 0.7626(5) 0.0382(6) Uani 1 1 d D U . . .
H14 H 1.099080 0.493088 0.716766 0.046 Uiso 1 1 calc R U . . .
C11 C 0.8493(7) 0.6132(4) 0.8991(5) 0.0388(6) Uani 1 1 d D U . . .
H11 H 0.787365 0.643409 0.944548 0.047 Uiso 1 1 calc R U . . .
C2 C 0.3586(9) 0.3639(4) 0.5638(5) 0.0404(17) Uani 1 1 d D U . . .
C7 C 0.3500(8) 0.7703(4) 0.6998(5) 0.0418(8) Uani 1 1 d D U . . .
H7 H 0.429748 0.807322 0.748889 0.050 Uiso 1 1 calc R U . . .
C1 C 0.6398(8) 0.3817(4) 0.7061(6) 0.0405(16) Uani 1 1 d D U . . .
C5 C 0.0829(8) 0.7484(4) 0.5771(5) 0.0433(9) Uani 1 1 d D U . . .
H5 H -0.019204 0.770805 0.544048 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2013(8) 0.8046(4) 0.6507(5) 0.0430(9) Uani 1 1 d D U . . .
H6 H 0.179393 0.864335 0.665953 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 1.998(4) . ?
Rh1 N1 2.076(4) . ?
Rh1 C2 1.874(5) . ?
Rh1 C1 1.833(6) . ?
Br1 C13 1.897(6) . ?
O3 C3 1.296(7) . ?
N1 C9 1.310(7) . ?
N1 C10 1.431(7) . ?
O2 C2 1.097(7) . ?
C8 C3 1.405(8) . ?
C8 C9 1.437(8) . ?
C8 C7 1.395(8) . ?
C3 C4 1.404(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.114(7) . ?
C13 C12 1.353(9) . ?
C13 C14 1.390(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.365(9) . ?
C15 C14 1.403(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(8) . ?
C10 C11 1.400(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.403(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.365(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 N1 90.19(19) . . ?
C2 Rh1 O3 88.4(2) . . ?
C2 Rh1 N1 178.34(19) . . ?
C1 Rh1 O3 171.9(3) . . ?
C1 Rh1 N1 95.3(2) . . ?
C1 Rh1 C2 86.2(3) . . ?
C3 O3 Rh1 129.8(4) . . ?
C9 N1 Rh1 122.8(4) . . ?
C9 N1 C10 115.4(5) . . ?
C10 N1 Rh1 121.9(4) . . ?
C3 C8 C9 123.7(5) . . ?
C7 C8 C3 120.2(5) . . ?
C7 C8 C9 116.0(5) . . ?
O3 C3 C8 124.4(5) . . ?
O3 C3 C4 118.3(5) . . ?
C4 C3 C8 117.3(5) . . ?
N1 C9 C8 128.6(5) . . ?
N1 C9 H9 115.7 . . ?
C8 C9 H9 115.7 . . ?
C12 C13 Br1 119.8(4) . . ?
C12 C13 C14 123.0(6) . . ?
C14 C13 Br1 117.3(5) . . ?
C10 C15 H15 119.3 . . ?
C10 C15 C14 121.5(5) . . ?
C14 C15 H15 119.3 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.4(5) . . ?
C5 C4 H4 119.3 . . ?
C15 C10 N1 119.6(4) . . ?
C15 C10 C11 120.2(5) . . ?
C11 C10 N1 120.1(6) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.6(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 C15 116.9(7) . . ?
C13 C14 H14 121.5 . . ?
C15 C14 H14 121.5 . . ?
C10 C11 C12 118.8(6) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
O2 C2 Rh1 177.1(8) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.4(6) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 175.6(7) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9(6) . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 118.7(6) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 2.6(11) . . . . ?
Rh1 O3 C3 C4 -177.7(5) . . . . ?
Rh1 N1 C9 C8 -5.6(10) . . . . ?
Rh1 N1 C10 C15 43.9(8) . . . . ?
Rh1 N1 C10 C11 -136.3(5) . . . . ?
Br1 C13 C12 C11 -179.4(4) . . . . ?
Br1 C13 C14 C15 178.6(4) . . . . ?
O3 C3 C4 C5 178.1(6) . . . . ?
N1 C10 C11 C12 -179.0(5) . . . . ?
C8 C3 C4 C5 -2.2(11) . . . . ?
C8 C7 C6 C5 -0.1(10) . . . . ?
C3 C8 C9 N1 -1.1(12) . . . . ?
C3 C8 C7 C6 -0.2(10) . . . . ?
C3 C4 C5 C6 2.0(11) . . . . ?
C9 N1 C10 C15 -137.4(6) . . . . ?
C9 N1 C10 C11 42.4(8) . . . . ?
C9 C8 C3 O3 3.0(11) . . . . ?
C9 C8 C3 C4 -176.7(7) . . . . ?
C9 C8 C7 C6 178.0(6) . . . . ?
C13 C12 C11 C10 -0.7(8) . . . . ?
C15 C10 C11 C12 0.9(8) . . . . ?
C4 C5 C6 C7 -0.8(9) . . . . ?
C10 N1 C9 C8 175.7(7) . . . . ?
C10 C15 C14 C13 2.2(10) . . . . ?
C12 C13 C14 C15 -2.1(10) . . . . ?
C14 C13 C12 C11 1.4(10) . . . . ?
C14 C15 C10 N1 178.2(5) . . . . ?
C14 C15 C10 C11 -1.7(10) . . . . ?
C7 C8 C3 O3 -179.0(6) . . . . ?
C7 C8 C3 C4 1.3(10) . . . . ?
C7 C8 C9 N1 -179.2(7) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.00164000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.852
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-05-HP-ESRF-1p50GPa
_database_code_depnum_ccdc_archive 'CCDC 2427934'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-05-HP-ESRF-1p50GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.449 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7378(6)
_cell_length_b                   14.7391(7)
_cell_length_c                   10.3776(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.360(6)
_cell_angle_gamma                90
_cell_volume                     1288.77(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1078
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.9470
_cell_measurement_theta_min      2.1930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.449
_diffrn_reflns_Laue_measured_fraction_max 0.387
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2940
_diffrn_reflns_point_group_measured_fraction_full 0.449
_diffrn_reflns_point_group_measured_fraction_max 0.387
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.793
_diffrn_reflns_theta_min         1.978
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.387
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0297862000
_diffrn_orient_matrix_UB_12      0.0151250000
_diffrn_orient_matrix_UB_13      0.0159722000
_diffrn_orient_matrix_UB_21      0.0263946000
_diffrn_orient_matrix_UB_22      -0.0065381000
_diffrn_orient_matrix_UB_23      0.0376735000
_diffrn_orient_matrix_UB_31      0.0278793000
_diffrn_orient_matrix_UB_32      0.0223637000
_diffrn_orient_matrix_UB_33      0.0002429000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1509
_reflns_number_total             1731
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1731
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0523P)²+2.7030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1128
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48005(7) 0.46184(3) 0.64078(4) 0.0324(2) Uani 1 1 d D U . . .
Br1 Br 1.32700(9) 0.55682(5) 0.95428(6) 0.0408(3) Uani 1 1 d D U . . .
O3 O 0.2850(7) 0.5385(3) 0.5820(4) 0.0372(13) Uani 1 1 d D U . . .
N1 N 0.6117(7) 0.5753(4) 0.7258(5) 0.0327(11) Uani 1 1 d D U . . .
O2 O 0.2923(9) 0.3018(4) 0.5118(5) 0.056(2) Uani 1 1 d D U . . .
C8 C 0.3842(9) 0.6810(4) 0.6805(6) 0.0373(9) Uani 1 1 d D U . . .
C3 C 0.2640(9) 0.6237(4) 0.6057(6) 0.0371(9) Uani 1 1 d D U . . .
C9 C 0.5459(9) 0.6539(4) 0.7340(6) 0.0335(15) Uani 1 1 d D U . . .
H9 H 0.613372 0.698452 0.781127 0.040 Uiso 1 1 calc R U . . .
O1 O 0.7299(9) 0.3247(4) 0.7433(6) 0.059(2) Uani 1 1 d D U . . .
C13 C 1.1032(8) 0.5645(4) 0.8848(6) 0.0343(7) Uani 1 1 d D U . . .
C15 C 0.8719(8) 0.5240(4) 0.7137(6) 0.0342(7) Uani 1 1 d D U . . .
H15 H 0.823683 0.494897 0.633820 0.041 Uiso 1 1 calc R U . . .
C4 C 0.1126(9) 0.6610(4) 0.5548(6) 0.0382(9) Uani 1 1 d D U . . .
H4 H 0.031677 0.624933 0.503727 0.046 Uiso 1 1 calc R U . . .
C10 C 0.7806(8) 0.5704(4) 0.7808(5) 0.0341(7) Uani 1 1 d D U . . .
C12 C 1.0155(8) 0.6103(4) 0.9523(5) 0.0347(7) Uani 1 1 d D U . . .
H12 H 1.064597 0.638966 1.032463 0.042 Uiso 1 1 calc R U . . .
C14 C 1.0359(8) 0.5203(4) 0.7642(6) 0.0344(7) Uani 1 1 d D U . . .
H14 H 1.098672 0.489288 0.719046 0.041 Uiso 1 1 calc R U . . .
C11 C 0.8503(8) 0.6148(4) 0.9015(5) 0.0346(7) Uani 1 1 d D U . . .
H11 H 0.788435 0.646355 0.946846 0.042 Uiso 1 1 calc R U . . .
C2 C 0.3587(10) 0.3610(4) 0.5608(6) 0.041(2) Uani 1 1 d D U . . .
C7 C 0.3490(9) 0.7716(4) 0.7024(6) 0.0380(9) Uani 1 1 d D U . . .
H7 H 0.428675 0.809170 0.751837 0.046 Uiso 1 1 calc R U . . .
C1 C 0.6405(9) 0.3794(4) 0.7044(6) 0.0355(18) Uani 1 1 d D U . . .
C5 C 0.0820(9) 0.7485(4) 0.5786(6) 0.0390(10) Uani 1 1 d D U . . .
H5 H -0.020242 0.771069 0.544846 0.047 Uiso 1 1 calc R U . . .
C6 C 0.1999(9) 0.8056(5) 0.6526(6) 0.0387(9) Uani 1 1 d D U . . .
H6 H 0.177453 0.865747 0.667671 0.046 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 2.001(5) . ?
Rh1 N1 2.089(5) . ?
Rh1 C2 1.886(6) . ?
Rh1 C1 1.841(6) . ?
Br1 C13 1.899(7) . ?
O3 C3 1.302(7) . ?
N1 C9 1.306(8) . ?
N1 C10 1.436(8) . ?
O2 C2 1.095(7) . ?
C8 C3 1.409(8) . ?
C8 C9 1.431(9) . ?
C8 C7 1.403(9) . ?
C3 C4 1.400(9) . ?
C9 H9 0.9300 . ?
O1 C1 1.120(8) . ?
C13 C12 1.349(10) . ?
C13 C14 1.395(7) . ?
C15 H15 0.9300 . ?
C15 C10 1.372(10) . ?
C15 C14 1.390(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.354(9) . ?
C10 C11 1.401(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.401(9) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.363(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(9) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 N1 90.3(2) . . ?
C2 Rh1 O3 88.7(3) . . ?
C2 Rh1 N1 178.7(2) . . ?
C1 Rh1 O3 171.4(3) . . ?
C1 Rh1 N1 95.5(3) . . ?
C1 Rh1 C2 85.6(3) . . ?
C3 O3 Rh1 129.7(4) . . ?
C9 N1 Rh1 122.3(5) . . ?
C9 N1 C10 116.3(5) . . ?
C10 N1 Rh1 121.4(4) . . ?
C3 C8 C9 124.2(6) . . ?
C7 C8 C3 119.8(6) . . ?
C7 C8 C9 116.0(6) . . ?
O3 C3 C8 124.1(6) . . ?
O3 C3 C4 118.3(5) . . ?
C4 C3 C8 117.7(6) . . ?
N1 C9 C8 128.9(6) . . ?
N1 C9 H9 115.5 . . ?
C8 C9 H9 115.5 . . ?
C12 C13 Br1 120.1(4) . . ?
C12 C13 C14 122.5(6) . . ?
C14 C13 Br1 117.4(6) . . ?
C10 C15 H15 119.7 . . ?
C10 C15 C14 120.6(5) . . ?
C14 C15 H15 119.7 . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.2(6) . . ?
C5 C4 H4 119.4 . . ?
C15 C10 N1 119.9(5) . . ?
C15 C10 C11 120.8(6) . . ?
C11 C10 N1 119.3(6) . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 119.9(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C14 H14 121.1 . . ?
C15 C14 C13 117.8(7) . . ?
C15 C14 H14 121.1 . . ?
C10 C11 H11 120.8 . . ?
C12 C11 C10 118.4(7) . . ?
C12 C11 H11 120.8 . . ?
O2 C2 Rh1 177.3(9) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 C8 121.1(6) . . ?
C6 C7 H7 119.4 . . ?
O1 C1 Rh1 175.0(8) . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.5(6) . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 118.7(6) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 1.1(12) . . . . ?
Rh1 O3 C3 C4 -178.5(6) . . . . ?
Rh1 N1 C9 C8 -5.9(11) . . . . ?
Rh1 N1 C10 C15 42.8(9) . . . . ?
Rh1 N1 C10 C11 -138.4(5) . . . . ?
Br1 C13 C12 C11 -179.2(4) . . . . ?
Br1 C13 C14 C15 178.9(5) . . . . ?
O3 C3 C4 C5 178.4(7) . . . . ?
N1 C10 C11 C12 -179.0(6) . . . . ?
C8 C3 C4 C5 -1.2(12) . . . . ?
C8 C7 C6 C5 -0.1(10) . . . . ?
C3 C8 C9 N1 -0.3(13) . . . . ?
C3 C8 C7 C6 0.0(11) . . . . ?
C3 C4 C5 C6 1.1(12) . . . . ?
C9 N1 C10 C15 -138.2(7) . . . . ?
C9 N1 C10 C11 40.6(9) . . . . ?
C9 C8 C3 O3 3.2(13) . . . . ?
C9 C8 C3 C4 -177.3(7) . . . . ?
C9 C8 C7 C6 178.0(7) . . . . ?
C13 C12 C11 C10 0.3(9) . . . . ?
C15 C10 C11 C12 -0.2(9) . . . . ?
C4 C5 C6 C7 -0.5(10) . . . . ?
C10 N1 C9 C8 175.1(7) . . . . ?
C10 C15 C14 C13 0.4(11) . . . . ?
C12 C13 C14 C15 -0.4(11) . . . . ?
C14 C13 C12 C11 0.0(10) . . . . ?
C14 C15 C10 N1 178.6(6) . . . . ?
C14 C15 C10 C11 -0.1(11) . . . . ?
C7 C8 C3 O3 -178.9(7) . . . . ?
C7 C8 C3 C4 0.6(11) . . . . ?
C7 C8 C9 N1 -178.3(7) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00372000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.115
_oxdiff_exptl_absorpt_empirical_full_min 0.841
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-09-HP-ESRF-3p75GPa
_database_code_depnum_ccdc_archive 'CCDC 2427935'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-09-HP-ESRF-3p75GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.450 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6599(6)
_cell_length_b                   14.4180(8)
_cell_length_c                   9.8517(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.531(6)
_cell_angle_gamma                90
_cell_volume                     1190.72(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    882
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.9920
_cell_measurement_theta_min      2.0390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.450
_diffrn_reflns_Laue_measured_fraction_max 0.386
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2665
_diffrn_reflns_point_group_measured_fraction_full 0.450
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.797
_diffrn_reflns_theta_min         2.041
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.450
_diffrn_measured_fraction_theta_max 0.386
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0289671000
_diffrn_orient_matrix_UB_12      0.0158505000
_diffrn_orient_matrix_UB_13      0.0175721000
_diffrn_orient_matrix_UB_21      0.0265053000
_diffrn_orient_matrix_UB_22      -0.0072285000
_diffrn_orient_matrix_UB_23      0.0391837000
_diffrn_orient_matrix_UB_31      0.0291023000
_diffrn_orient_matrix_UB_32      0.0224272000
_diffrn_orient_matrix_UB_33      0.0000721000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1404
_reflns_number_total             1593
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1593
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0565P)²+2.4646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1037
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47944(6) 0.45893(3) 0.63852(4) 0.02349(17) Uani 1 1 d D U . . .
Br1 Br 1.33138(8) 0.55534(4) 0.96141(6) 0.0277(2) Uani 1 1 d D U . . .
O3 O 0.2794(6) 0.5345(3) 0.5871(4) 0.0289(11) Uani 1 1 d D U . . .
N1 N 0.6100(7) 0.5737(3) 0.7291(5) 0.0247(10) Uani 1 1 d D U . . .
O2 O 0.2877(8) 0.2975(4) 0.5018(5) 0.0441(19) Uani 1 1 d D U . . .
C8 C 0.3809(8) 0.6814(4) 0.6857(6) 0.0249(8) Uani 1 1 d D U . . .
C3 C 0.2587(8) 0.6229(4) 0.6103(6) 0.0252(8) Uani 1 1 d D U . . .
C9 C 0.5417(8) 0.6535(4) 0.7416(5) 0.0251(13) Uani 1 1 d D U . . .
H9 H 0.607942 0.698028 0.794624 0.030 Uiso 1 1 calc R U . . .
O1 O 0.7297(8) 0.3172(4) 0.7378(6) 0.0474(19) Uani 1 1 d D U . . .
C13 C 1.1059(8) 0.5640(4) 0.8904(5) 0.0250(6) Uani 1 1 d D U . . .
C15 C 0.8732(8) 0.5201(4) 0.7161(6) 0.0255(7) Uani 1 1 d D U . . .
H15 H 0.825023 0.488614 0.634037 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1050(9) 0.6606(4) 0.5566(6) 0.0266(8) Uani 1 1 d D U . . .
H4 H 0.024355 0.623518 0.503398 0.032 Uiso 1 1 calc R U . . .
C10 C 0.7800(8) 0.5709(4) 0.7847(5) 0.0254(7) Uani 1 1 d D U . . .
C12 C 1.0186(8) 0.6151(4) 0.9589(5) 0.0256(7) Uani 1 1 d D U . . .
H12 H 1.068450 0.646508 1.040612 0.031 Uiso 1 1 calc R U . . .
C14 C 1.0379(8) 0.5155(4) 0.7682(6) 0.0253(7) Uani 1 1 d D U . . .
H14 H 1.100544 0.481002 0.722718 0.030 Uiso 1 1 calc R U . . .
C11 C 0.8541(8) 0.6206(4) 0.9069(5) 0.0256(7) Uani 1 1 d D U . . .
H11 H 0.793439 0.656758 0.952351 0.031 Uiso 1 1 calc R U . . .
C2 C 0.3562(9) 0.3573(4) 0.5533(6) 0.0314(18) Uani 1 1 d D U . . .
C7 C 0.3440(8) 0.7741(4) 0.7095(6) 0.0257(8) Uani 1 1 d D U . . .
H7 H 0.423691 0.812612 0.760739 0.031 Uiso 1 1 calc R U . . .
C1 C 0.6407(9) 0.3747(4) 0.6991(6) 0.0296(17) Uani 1 1 d D U . . .
C5 C 0.0736(9) 0.7505(4) 0.5818(6) 0.0274(8) Uani 1 1 d D U . . .
H5 H -0.029097 0.773579 0.547252 0.033 Uiso 1 1 calc R U . . .
C6 C 0.1928(8) 0.8089(4) 0.6586(5) 0.0268(8) Uani 1 1 d D U . . .
H6 H 0.170098 0.870360 0.674984 0.032 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.0768(10) 3_666 ?
Rh1 O3 2.001(5) . ?
Rh1 N1 2.075(5) . ?
Rh1 C2 1.881(6) . ?
Rh1 C1 1.834(6) . ?
Br1 C13 1.906(6) . ?
O3 C3 1.315(7) . ?
N1 C9 1.313(8) . ?
N1 C10 1.437(8) . ?
O2 C2 1.096(7) . ?
C8 C3 1.409(8) . ?
C8 C9 1.421(8) . ?
C8 C7 1.408(8) . ?
C3 C4 1.412(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.131(7) . ?
C13 C12 1.351(9) . ?
C13 C14 1.389(7) . ?
C15 H15 0.9300 . ?
C15 C10 1.385(9) . ?
C15 C14 1.391(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.360(8) . ?
C10 C11 1.410(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.390(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.374(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.398(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 81.45(17) . 3_666 ?
O3 Rh1 N1 91.03(19) . . ?
N1 Rh1 Rh1 84.42(15) . 3_666 ?
C2 Rh1 Rh1 94.7(2) . 3_666 ?
C2 Rh1 O3 87.3(3) . . ?
C2 Rh1 N1 178.2(2) . . ?
C1 Rh1 Rh1 107.2(3) . 3_666 ?
C1 Rh1 O3 169.5(3) . . ?
C1 Rh1 N1 95.8(2) . . ?
C1 Rh1 C2 86.0(3) . . ?
C3 O3 Rh1 129.1(4) . . ?
C9 N1 Rh1 121.9(4) . . ?
C9 N1 C10 115.6(5) . . ?
C10 N1 Rh1 122.5(4) . . ?
C3 C8 C9 124.6(5) . . ?
C7 C8 C3 118.9(5) . . ?
C7 C8 C9 116.5(5) . . ?
O3 C3 C8 123.6(5) . . ?
O3 C3 C4 117.7(5) . . ?
C8 C3 C4 118.7(5) . . ?
N1 C9 C8 129.2(5) . . ?
N1 C9 H9 115.4 . . ?
C8 C9 H9 115.4 . . ?
C12 C13 Br1 120.2(4) . . ?
C12 C13 C14 122.6(6) . . ?
C14 C13 Br1 117.2(5) . . ?
C10 C15 H15 119.5 . . ?
C10 C15 C14 120.9(5) . . ?
C14 C15 H15 119.5 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C15 C10 N1 119.7(5) . . ?
C15 C10 C11 119.3(6) . . ?
C11 C10 N1 121.0(6) . . ?
C13 C12 H12 120.1 . . ?
C13 C12 C11 119.8(5) . . ?
C11 C12 H12 120.1 . . ?
C13 C14 C15 117.9(6) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.3(6) . . ?
C12 C11 H11 120.3 . . ?
O2 C2 Rh1 178.0(9) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.4(5) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 173.8(8) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(6) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 118.9(6) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -3.1(10) . . . . ?
Rh1 O3 C3 C4 177.0(5) . . . . ?
Rh1 N1 C9 C8 -8.3(10) . . . . ?
Rh1 N1 C10 C15 38.1(8) . . . . ?
Rh1 N1 C10 C11 -143.1(5) . . . . ?
Br1 C13 C12 C11 -179.6(4) . . . . ?
Br1 C13 C14 C15 179.1(5) . . . . ?
O3 C3 C4 C5 177.2(6) . . . . ?
N1 C10 C11 C12 179.0(6) . . . . ?
C8 C3 C4 C5 -2.6(11) . . . . ?
C8 C7 C6 C5 0.1(9) . . . . ?
C3 C8 C9 N1 4.3(12) . . . . ?
C3 C8 C7 C6 -1.3(10) . . . . ?
C3 C4 C5 C6 1.5(10) . . . . ?
C9 N1 C10 C15 -143.1(6) . . . . ?
C9 N1 C10 C11 35.7(8) . . . . ?
C9 C8 C3 O3 2.2(11) . . . . ?
C9 C8 C3 C4 -177.9(7) . . . . ?
C9 C8 C7 C6 179.1(6) . . . . ?
C13 C12 C11 C10 1.4(8) . . . . ?
C15 C10 C11 C12 -2.2(8) . . . . ?
C4 C5 C6 C7 -0.2(9) . . . . ?
C10 N1 C9 C8 172.9(7) . . . . ?
C10 C15 C14 C13 -0.5(10) . . . . ?
C12 C13 C14 C15 -0.3(10) . . . . ?
C14 C13 C12 C11 -0.2(10) . . . . ?
C14 C15 C10 N1 -179.4(6) . . . . ?
C14 C15 C10 C11 1.8(10) . . . . ?
C7 C8 C3 O3 -177.4(6) . . . . ?
C7 C8 C3 C4 2.5(10) . . . . ?
C7 C8 C9 N1 -176.1(7) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.03070000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.605
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-10-HP-ESRF-4p55GPa
_database_code_depnum_ccdc_archive 'CCDC 2427937'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-10-HP-ESRF-4p55GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.449 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6186(5)
_cell_length_b                   14.3215(6)
_cell_length_c                   9.7119(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.320(5)
_cell_angle_gamma                90
_cell_volume                     1161.51(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    912
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.0870
_cell_measurement_theta_min      2.0950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.449
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2601
_diffrn_reflns_point_group_measured_fraction_full 0.449
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.795
_diffrn_reflns_theta_min         2.060
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0290471000
_diffrn_orient_matrix_UB_12      0.0158359000
_diffrn_orient_matrix_UB_13      0.0181812000
_diffrn_orient_matrix_UB_21      0.0269091000
_diffrn_orient_matrix_UB_22      -0.0072480000
_diffrn_orient_matrix_UB_23      0.0395374000
_diffrn_orient_matrix_UB_31      0.0289529000
_diffrn_orient_matrix_UB_32      0.0226735000
_diffrn_orient_matrix_UB_33      -0.0001498000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1375
_reflns_number_total             1543
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0467P)²+3.2715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0977
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47941(7) 0.45824(3) 0.63808(4) 0.02216(17) Uani 1 1 d D U . . .
Br1 Br 1.33226(8) 0.55510(4) 0.96320(6) 0.0257(2) Uani 1 1 d D U . . .
O3 O 0.2782(6) 0.5340(3) 0.5889(5) 0.0273(11) Uani 1 1 d D U . . .
N1 N 0.6104(7) 0.5745(3) 0.7294(5) 0.0223(10) Uani 1 1 d D U . . .
O2 O 0.2856(8) 0.2967(4) 0.4994(5) 0.0398(18) Uani 1 1 d D U . . .
C8 C 0.3797(8) 0.6826(4) 0.6865(6) 0.0241(8) Uani 1 1 d D U . . .
C3 C 0.2576(8) 0.6229(4) 0.6111(6) 0.0244(8) Uani 1 1 d D U . . .
C9 C 0.5421(8) 0.6536(4) 0.7427(6) 0.0229(13) Uani 1 1 d D U . . .
H9 H 0.608734 0.698281 0.796753 0.028 Uiso 1 1 calc R U . . .
O1 O 0.7306(8) 0.3165(4) 0.7370(6) 0.0437(19) Uani 1 1 d D U . . .
C13 C 1.1083(8) 0.5628(4) 0.8912(6) 0.0236(7) Uani 1 1 d D U . . .
C15 C 0.8719(8) 0.5191(4) 0.7169(6) 0.0236(7) Uani 1 1 d D U . . .
H15 H 0.822816 0.487601 0.633845 0.028 Uiso 1 1 calc R U . . .
C4 C 0.1029(9) 0.6608(4) 0.5580(6) 0.0257(8) Uani 1 1 d D U . . .
H4 H 0.021233 0.623293 0.505756 0.031 Uiso 1 1 calc R U . . .
C10 C 0.7804(8) 0.5702(4) 0.7858(6) 0.0235(7) Uani 1 1 d D U . . .
C12 C 1.0200(8) 0.6167(4) 0.9594(5) 0.0238(7) Uani 1 1 d D U . . .
H12 H 1.070053 0.650068 1.040306 0.029 Uiso 1 1 calc R U . . .
C14 C 1.0379(8) 0.5135(4) 0.7691(6) 0.0238(7) Uani 1 1 d D U . . .
H14 H 1.099471 0.477548 0.722989 0.029 Uiso 1 1 calc R U . . .
C11 C 0.8540(8) 0.6213(4) 0.9070(5) 0.0239(7) Uani 1 1 d D U . . .
H11 H 0.792870 0.658088 0.952345 0.029 Uiso 1 1 calc R U . . .
C2 C 0.3572(9) 0.3559(4) 0.5516(6) 0.0276(17) Uani 1 1 d D U . . .
C7 C 0.3435(8) 0.7760(4) 0.7104(6) 0.0250(8) Uani 1 1 d D U . . .
H7 H 0.423390 0.814946 0.761858 0.030 Uiso 1 1 calc R U . . .
C1 C 0.6413(9) 0.3739(4) 0.6981(6) 0.0275(17) Uani 1 1 d D U . . .
C5 C 0.0726(9) 0.7511(4) 0.5823(6) 0.0266(8) Uani 1 1 d D U . . .
H5 H -0.030193 0.774661 0.547324 0.032 Uiso 1 1 calc R U . . .
C6 C 0.1929(8) 0.8100(4) 0.6592(6) 0.0262(8) Uani 1 1 d D U . . .
H6 H 0.170045 0.871895 0.675085 0.031 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.0366(10) 3_666 ?
Rh1 O3 2.000(5) . ?
Rh1 N1 2.083(5) . ?
Rh1 C2 1.877(6) . ?
Rh1 C1 1.828(6) . ?
Br1 C13 1.886(6) . ?
O3 C3 1.311(7) . ?
N1 C9 1.298(8) . ?
N1 C10 1.433(8) . ?
O2 C2 1.097(7) . ?
C8 C3 1.412(8) . ?
C8 C9 1.432(8) . ?
C8 C7 1.406(8) . ?
C3 C4 1.413(9) . ?
C9 H9 0.9300 . ?
O1 C1 1.126(7) . ?
C13 C12 1.364(10) . ?
C13 C14 1.385(7) . ?
C15 H15 0.9300 . ?
C15 C10 1.365(10) . ?
C15 C14 1.397(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.352(8) . ?
C10 C11 1.398(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.397(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.360(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.400(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 81.92(17) . 3_666 ?
O3 Rh1 N1 90.84(19) . . ?
N1 Rh1 Rh1 83.78(15) . 3_666 ?
C2 Rh1 Rh1 95.0(2) . 3_666 ?
C2 Rh1 O3 87.7(2) . . ?
C2 Rh1 N1 178.2(2) . . ?
C1 Rh1 Rh1 107.2(3) . 3_666 ?
C1 Rh1 O3 169.2(3) . . ?
C1 Rh1 N1 95.8(2) . . ?
C1 Rh1 C2 85.8(3) . . ?
C3 O3 Rh1 129.2(4) . . ?
C9 N1 Rh1 122.0(4) . . ?
C9 N1 C10 116.5(5) . . ?
C10 N1 Rh1 121.5(4) . . ?
C3 C8 C9 123.7(5) . . ?
C7 C8 C3 119.6(6) . . ?
C7 C8 C9 116.6(5) . . ?
O3 C3 C8 124.0(5) . . ?
O3 C3 C4 117.9(5) . . ?
C8 C3 C4 118.1(5) . . ?
N1 C9 C8 129.7(5) . . ?
N1 C9 H9 115.1 . . ?
C8 C9 H9 115.1 . . ?
C12 C13 Br1 119.7(4) . . ?
C12 C13 C14 121.6(6) . . ?
C14 C13 Br1 118.6(5) . . ?
C10 C15 H15 119.4 . . ?
C10 C15 C14 121.1(5) . . ?
C14 C15 H15 119.4 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C15 C10 N1 119.7(5) . . ?
C15 C10 C11 119.7(6) . . ?
C11 C10 N1 120.5(6) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.6(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 C15 118.3(7) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11 120.2 . . ?
O2 C2 Rh1 179.1(6) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 C8 120.7(5) . . ?
C6 C7 H7 119.6 . . ?
O1 C1 Rh1 173.7(8) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.3(6) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -4.6(10) . . . . ?
Rh1 O3 C3 C4 176.3(5) . . . . ?
Rh1 N1 C9 C8 -8.8(10) . . . . ?
Rh1 N1 C10 C15 38.6(8) . . . . ?
Rh1 N1 C10 C11 -144.4(5) . . . . ?
Br1 C13 C12 C11 -179.2(4) . . . . ?
Br1 C13 C14 C15 179.6(5) . . . . ?
O3 C3 C4 C5 177.4(6) . . . . ?
N1 C10 C11 C12 -179.5(6) . . . . ?
C8 C3 C4 C5 -1.7(11) . . . . ?
C8 C7 C6 C5 0.3(10) . . . . ?
C3 C8 C9 N1 5.0(12) . . . . ?
C3 C8 C7 C6 -1.4(10) . . . . ?
C3 C4 C5 C6 0.7(11) . . . . ?
C9 N1 C10 C15 -143.6(7) . . . . ?
C9 N1 C10 C11 33.4(8) . . . . ?
C9 C8 C3 O3 2.6(12) . . . . ?
C9 C8 C3 C4 -178.3(7) . . . . ?
C9 C8 C7 C6 179.0(6) . . . . ?
C13 C12 C11 C10 0.4(8) . . . . ?
C15 C10 C11 C12 -2.5(9) . . . . ?
C4 C5 C6 C7 0.1(10) . . . . ?
C10 N1 C9 C8 173.4(7) . . . . ?
C10 C15 C14 C13 -1.4(10) . . . . ?
C12 C13 C14 C15 -0.7(10) . . . . ?
C14 C13 C12 C11 1.1(10) . . . . ?
C14 C15 C10 N1 180.0(6) . . . . ?
C14 C15 C10 C11 3.0(10) . . . . ?
C7 C8 C3 O3 -177.0(7) . . . . ?
C7 C8 C3 C4 2.1(10) . . . . ?
C7 C8 C9 N1 -175.4(7) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.03298000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.683
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-15-HP-ESRF-7p34GPa
_database_code_depnum_ccdc_archive 'CCDC 2427942'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-15-HP-ESRF-7p34GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.445 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4973(5)
_cell_length_b                   14.1187(9)
_cell_length_c                   9.3456(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.474(6)
_cell_angle_gamma                90
_cell_volume                     1090.34(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    738
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.0910
_cell_measurement_theta_min      2.1290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.445
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2408
_diffrn_reflns_point_group_measured_fraction_full 0.445
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.800
_diffrn_reflns_theta_min         2.105
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.445
_diffrn_measured_fraction_theta_max 0.379
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0290102000
_diffrn_orient_matrix_UB_12      0.0161636000
_diffrn_orient_matrix_UB_13      -0.0196386000
_diffrn_orient_matrix_UB_21      -0.0282946000
_diffrn_orient_matrix_UB_22      -0.0066951000
_diffrn_orient_matrix_UB_23      -0.0405153000
_diffrn_orient_matrix_UB_31      -0.0285113000
_diffrn_orient_matrix_UB_32      0.0231185000
_diffrn_orient_matrix_UB_33      0.0020029000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1325
_reflns_number_total             1438
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1438
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0413
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0632P)²+4.7025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1247
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47959(8) 0.45666(4) 0.63736(6) 0.0261(2) Uani 1 1 d D U . . .
Br1 Br 1.33519(10) 0.55423(5) 0.96755(8) 0.0281(3) Uani 1 1 d D U . . .
O3 O 0.2760(8) 0.5321(4) 0.5915(6) 0.0310(14) Uani 1 1 d D U . . .
N1 N 0.6087(8) 0.5741(4) 0.7300(6) 0.0248(11) Uani 1 1 d D U . . .
O2 O 0.2792(9) 0.2954(4) 0.4949(7) 0.040(2) Uani 1 1 d D U . . .
C8 C 0.3767(10) 0.6819(5) 0.6887(8) 0.0286(10) Uani 1 1 d D U . . .
C3 C 0.2526(10) 0.6208(5) 0.6126(8) 0.0284(10) Uani 1 1 d D U . . .
C9 C 0.5402(9) 0.6536(5) 0.7464(7) 0.0251(16) Uani 1 1 d D U . . .
H9 H 0.606435 0.698565 0.803544 0.030 Uiso 1 1 calc R U . . .
O1 O 0.7347(9) 0.3142(5) 0.7345(7) 0.042(2) Uani 1 1 d D U . . .
C13 C 1.1105(9) 0.5629(5) 0.8943(7) 0.0276(8) Uani 1 1 d D U . . .
C15 C 0.8726(9) 0.5151(5) 0.7205(7) 0.0276(8) Uani 1 1 d D U . . .
H15 H 0.822194 0.479492 0.639025 0.033 Uiso 1 1 calc R U . . .
C4 C 0.0970(10) 0.6588(5) 0.5595(8) 0.0293(10) Uani 1 1 d D U . . .
H4 H 0.014105 0.620220 0.508241 0.035 Uiso 1 1 calc R U . . .
C10 C 0.7818(9) 0.5719(5) 0.7858(7) 0.0277(8) Uani 1 1 d D U . . .
C12 C 1.0213(9) 0.6204(5) 0.9618(7) 0.0280(8) Uani 1 1 d D U . . .
H12 H 1.071556 0.655978 1.043402 0.034 Uiso 1 1 calc R U . . .
C14 C 1.0391(9) 0.5087(5) 0.7721(7) 0.0276(8) Uani 1 1 d D U . . .
H14 H 1.100779 0.469530 0.726660 0.033 Uiso 1 1 calc R U . . .
C11 C 0.8543(9) 0.6255(5) 0.9078(7) 0.0281(8) Uani 1 1 d D U . . .
H11 H 0.792023 0.664387 0.953069 0.034 Uiso 1 1 calc R U . . .
C2 C 0.3554(11) 0.3529(5) 0.5493(9) 0.033(2) Uani 1 1 d D U . . .
C7 C 0.3385(10) 0.7759(5) 0.7124(8) 0.0294(10) Uani 1 1 d D U . . .
H7 H 0.418351 0.815381 0.766349 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6435(10) 0.3718(5) 0.6954(8) 0.0264(18) Uani 1 1 d D U . . .
C5 C 0.0664(10) 0.7516(5) 0.5825(8) 0.0301(10) Uani 1 1 d D U . . .
H5 H -0.037356 0.775372 0.546582 0.036 Uiso 1 1 calc R U . . .
C6 C 0.1872(10) 0.8113(6) 0.6585(7) 0.0302(10) Uani 1 1 d D U . . .
H6 H 0.164999 0.874663 0.672474 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9368(13) 3_666 ?
Rh1 O3 1.991(6) . ?
Rh1 N1 2.064(6) . ?
Rh1 C2 1.879(7) . ?
Rh1 C1 1.821(7) . ?
Br1 C13 1.876(7) . ?
O3 C3 1.291(9) . ?
N1 C9 1.290(10) . ?
N1 C10 1.441(9) . ?
O2 C2 1.087(8) . ?
C8 C3 1.419(9) . ?
C8 C9 1.425(9) . ?
C8 C7 1.396(10) . ?
C3 C4 1.406(10) . ?
C9 H9 0.9300 . ?
O1 C1 1.125(9) . ?
C13 C12 1.361(11) . ?
C13 C14 1.391(8) . ?
C15 H15 0.9300 . ?
C15 C10 1.352(11) . ?
C15 C14 1.387(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(10) . ?
C10 C11 1.388(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.393(9) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.361(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(9) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.1(2) . 3_666 ?
O3 Rh1 N1 90.6(2) . . ?
N1 Rh1 Rh1 82.67(18) . 3_666 ?
C2 Rh1 Rh1 96.4(3) . 3_666 ?
C2 Rh1 O3 87.2(3) . . ?
C2 Rh1 N1 177.7(3) . . ?
C1 Rh1 Rh1 107.3(3) . 3_666 ?
C1 Rh1 O3 169.0(4) . . ?
C1 Rh1 N1 96.2(3) . . ?
C1 Rh1 C2 86.0(3) . . ?
C3 O3 Rh1 130.0(5) . . ?
C9 N1 Rh1 122.6(5) . . ?
C9 N1 C10 115.3(6) . . ?
C10 N1 Rh1 122.1(5) . . ?
C3 C8 C9 124.3(7) . . ?
C7 C8 C3 119.0(7) . . ?
C7 C8 C9 116.7(6) . . ?
O3 C3 C8 123.0(7) . . ?
O3 C3 C4 118.8(6) . . ?
C4 C3 C8 118.2(6) . . ?
N1 C9 C8 128.8(6) . . ?
N1 C9 H9 115.6 . . ?
C8 C9 H9 115.6 . . ?
C12 C13 Br1 119.9(4) . . ?
C12 C13 C14 121.7(7) . . ?
C14 C13 Br1 118.4(6) . . ?
C10 C15 H15 119.2 . . ?
C10 C15 C14 121.7(6) . . ?
C14 C15 H15 119.2 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(6) . . ?
C5 C4 H4 119.7 . . ?
C15 C10 N1 119.5(6) . . ?
C15 C10 C11 120.2(7) . . ?
C11 C10 N1 120.3(7) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.6(6) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 H14 121.2 . . ?
C15 C14 C13 117.6(8) . . ?
C15 C14 H14 121.2 . . ?
C10 C11 C12 119.3(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
O2 C2 Rh1 177.1(7) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.6(6) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 Rh1 173.8(9) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.3(7) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.2(7) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -5.5(13) . . . . ?
Rh1 O3 C3 C4 175.1(6) . . . . ?
Rh1 N1 C9 C8 -10.2(12) . . . . ?
Rh1 N1 C10 C15 32.4(10) . . . . ?
Rh1 N1 C10 C11 -145.9(6) . . . . ?
Br1 C13 C12 C11 -179.2(5) . . . . ?
Br1 C13 C14 C15 179.3(6) . . . . ?
O3 C3 C4 C5 178.5(8) . . . . ?
N1 C10 C11 C12 178.5(7) . . . . ?
C8 C3 C4 C5 -0.9(13) . . . . ?
C8 C7 C6 C5 2.3(11) . . . . ?
C3 C8 C9 N1 7.1(15) . . . . ?
C3 C8 C7 C6 -3.1(12) . . . . ?
C3 C4 C5 C6 0.1(13) . . . . ?
C9 N1 C10 C15 -149.7(8) . . . . ?
C9 N1 C10 C11 32.0(10) . . . . ?
C9 C8 C3 O3 1.7(14) . . . . ?
C9 C8 C3 C4 -179.0(8) . . . . ?
C9 C8 C7 C6 178.1(8) . . . . ?
C13 C12 C11 C10 -0.1(10) . . . . ?
C15 C10 C11 C12 0.2(10) . . . . ?
C4 C5 C6 C7 -0.7(11) . . . . ?
C10 N1 C9 C8 171.9(8) . . . . ?
C10 C15 C14 C13 0.0(13) . . . . ?
C12 C13 C14 C15 0.1(13) . . . . ?
C14 C13 C12 C11 0.0(12) . . . . ?
C14 C15 C10 N1 -178.4(7) . . . . ?
C14 C15 C10 C11 -0.2(13) . . . . ?
C7 C8 C3 O3 -177.0(8) . . . . ?
C7 C8 C3 C4 2.3(13) . . . . ?
C7 C8 C9 N1 -174.1(8) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.03889000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.284
_oxdiff_exptl_absorpt_empirical_full_min 0.695
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-06-HP-ESRF-2p03GPa
_database_code_depnum_ccdc_archive 'CCDC 2427940'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-06-HP-ESRF-2p03GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.450 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7263(5)
_cell_length_b                   14.6576(6)
_cell_length_c                   10.2270(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.111(5)
_cell_angle_gamma                90
_cell_volume                     1262.87(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1043
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.0990
_cell_measurement_theta_min      2.2030
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.450
_diffrn_reflns_Laue_measured_fraction_max 0.385
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2850
_diffrn_reflns_point_group_measured_fraction_full 0.450
_diffrn_reflns_point_group_measured_fraction_max 0.385
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.794
_diffrn_reflns_theta_min         1.995
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.450
_diffrn_measured_fraction_theta_max 0.385
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286755000
_diffrn_orient_matrix_UB_12      0.0157042000
_diffrn_orient_matrix_UB_13      -0.0167537000
_diffrn_orient_matrix_UB_21      -0.0260740000
_diffrn_orient_matrix_UB_22      -0.0073513000
_diffrn_orient_matrix_UB_23      -0.0379311000
_diffrn_orient_matrix_UB_31      -0.0294025000
_diffrn_orient_matrix_UB_32      0.0218771000
_diffrn_orient_matrix_UB_33      -0.0006272000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1495
_reflns_number_total             1689
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1689
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+3.5885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1184
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47968(7) 0.46090(3) 0.64016(5) 0.02821(19) Uani 1 1 d D U . . .
Br1 Br 1.32831(9) 0.55635(5) 0.95634(7) 0.0346(2) Uani 1 1 d D U . . .
O3 O 0.2823(7) 0.5371(3) 0.5834(5) 0.0344(14) Uani 1 1 d D U . . .
N1 N 0.6102(7) 0.5751(4) 0.7263(5) 0.0287(11) Uani 1 1 d D U . . .
O2 O 0.2909(9) 0.3001(4) 0.5083(6) 0.051(2) Uani 1 1 d D U . . .
C8 C 0.3834(9) 0.6812(4) 0.6820(6) 0.0314(9) Uani 1 1 d D U . . .
C3 C 0.2622(9) 0.6231(4) 0.6074(6) 0.0316(9) Uani 1 1 d D U . . .
C9 C 0.5460(9) 0.6539(4) 0.7359(6) 0.0293(15) Uani 1 1 d D U . . .
H9 H 0.613804 0.698391 0.783812 0.035 Uiso 1 1 calc R U . . .
O1 O 0.7291(9) 0.3224(5) 0.7416(7) 0.055(2) Uani 1 1 d D U . . .
C13 C 1.1041(8) 0.5634(5) 0.8865(6) 0.0294(7) Uani 1 1 d D U . . .
C15 C 0.8721(8) 0.5227(5) 0.7143(6) 0.0298(7) Uani 1 1 d D U . . .
H15 H 0.824000 0.492744 0.633870 0.036 Uiso 1 1 calc R U . . .
C4 C 0.1111(10) 0.6611(5) 0.5552(7) 0.0324(9) Uani 1 1 d D U . . .
H4 H 0.030629 0.625148 0.502320 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7801(8) 0.5706(5) 0.7822(6) 0.0298(7) Uani 1 1 d D U . . .
C12 C 1.0165(8) 0.6127(4) 0.9548(6) 0.0301(7) Uani 1 1 d D U . . .
H12 H 1.065495 0.643231 1.034418 0.036 Uiso 1 1 calc R U . . .
C14 C 1.0364(8) 0.5189(5) 0.7656(6) 0.0297(7) Uani 1 1 d D U . . .
H14 H 1.099122 0.487380 0.719899 0.036 Uiso 1 1 calc R U . . .
C11 C 0.8524(8) 0.6160(4) 0.9027(6) 0.0301(7) Uani 1 1 d D U . . .
H11 H 0.790743 0.648532 0.948276 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3578(10) 0.3604(5) 0.5580(7) 0.037(2) Uani 1 1 d D U . . .
C7 C 0.3462(9) 0.7727(5) 0.7047(6) 0.0323(9) Uani 1 1 d D U . . .
H7 H 0.425456 0.810527 0.754974 0.039 Uiso 1 1 calc R U . . .
C1 C 0.6392(10) 0.3790(5) 0.7033(7) 0.0328(18) Uani 1 1 d D U . . .
C5 C 0.0791(9) 0.7501(5) 0.5802(6) 0.0332(9) Uani 1 1 d D U . . .
H5 H -0.023098 0.772881 0.546768 0.040 Uiso 1 1 calc R U . . .
C6 C 0.1980(9) 0.8066(5) 0.6552(6) 0.0330(9) Uani 1 1 d D U . . .
H6 H 0.176003 0.867091 0.671197 0.040 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.1919(12) 3_666 ?
Rh1 O3 2.007(5) . ?
Rh1 N1 2.087(5) . ?
Rh1 C2 1.882(6) . ?
Rh1 C1 1.824(6) . ?
Br1 C13 1.903(7) . ?
O3 C3 1.305(8) . ?
N1 C9 1.298(8) . ?
N1 C10 1.444(8) . ?
O2 C2 1.107(8) . ?
C8 C3 1.417(9) . ?
C8 C9 1.438(9) . ?
C8 C7 1.413(9) . ?
C3 C4 1.403(9) . ?
C9 H9 0.9300 . ?
O1 C1 1.139(8) . ?
C13 C12 1.369(10) . ?
C13 C14 1.386(7) . ?
C15 H15 0.9300 . ?
C15 C10 1.382(10) . ?
C15 C14 1.394(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(9) . ?
C10 C11 1.398(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.392(9) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.354(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(9) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 80.11(19) . 3_666 ?
O3 Rh1 N1 90.5(2) . . ?
N1 Rh1 Rh1 85.10(17) . 3_666 ?
C2 Rh1 Rh1 93.6(3) . 3_666 ?
C2 Rh1 O3 87.9(3) . . ?
C2 Rh1 N1 178.1(2) . . ?
C1 Rh1 Rh1 107.5(3) . 3_666 ?
C1 Rh1 O3 170.6(4) . . ?
C1 Rh1 N1 95.5(3) . . ?
C1 Rh1 C2 86.2(3) . . ?
C3 O3 Rh1 129.1(4) . . ?
C9 N1 Rh1 123.1(5) . . ?
C9 N1 C10 115.4(6) . . ?
C10 N1 Rh1 121.4(4) . . ?
C3 C8 C9 124.2(6) . . ?
C7 C8 C3 119.2(6) . . ?
C7 C8 C9 116.6(6) . . ?
O3 C3 C8 124.3(6) . . ?
O3 C3 C4 118.2(6) . . ?
C4 C3 C8 117.5(6) . . ?
N1 C9 C8 128.4(6) . . ?
N1 C9 H9 115.8 . . ?
C8 C9 H9 115.8 . . ?
C12 C13 Br1 119.6(4) . . ?
C12 C13 C14 122.6(6) . . ?
C14 C13 Br1 117.8(6) . . ?
C10 C15 H15 119.8 . . ?
C10 C15 C14 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.6(6) . . ?
C5 C4 H4 119.2 . . ?
C15 C10 N1 119.7(5) . . ?
C15 C10 C11 119.8(6) . . ?
C11 C10 N1 120.5(7) . . ?
C13 C12 H12 120.7 . . ?
C13 C12 C11 118.6(6) . . ?
C11 C12 H12 120.7 . . ?
C13 C14 C15 118.3(7) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.2(7) . . ?
C12 C11 H11 119.9 . . ?
O2 C2 Rh1 177.3(9) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.7(6) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 Rh1 174.2(8) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(6) . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 119.3(6) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 0.1(12) . . . . ?
Rh1 O3 C3 C4 179.6(6) . . . . ?
Rh1 N1 C9 C8 -6.0(11) . . . . ?
Rh1 N1 C10 C15 41.7(9) . . . . ?
Rh1 N1 C10 C11 -139.6(5) . . . . ?
Br1 C13 C12 C11 -179.3(4) . . . . ?
Br1 C13 C14 C15 179.2(5) . . . . ?
O3 C3 C4 C5 177.6(7) . . . . ?
N1 C10 C11 C12 -178.9(6) . . . . ?
C8 C3 C4 C5 -2.9(12) . . . . ?
C8 C7 C6 C5 0.1(10) . . . . ?
C3 C8 C9 N1 0.6(13) . . . . ?
C3 C8 C7 C6 -1.0(11) . . . . ?
C3 C4 C5 C6 2.1(12) . . . . ?
C9 N1 C10 C15 -139.5(7) . . . . ?
C9 N1 C10 C11 39.1(9) . . . . ?
C9 C8 C3 O3 2.8(13) . . . . ?
C9 C8 C3 C4 -176.6(8) . . . . ?
C9 C8 C7 C6 178.0(7) . . . . ?
C13 C12 C11 C10 -0.7(9) . . . . ?
C15 C10 C11 C12 -0.3(9) . . . . ?
C4 C5 C6 C7 -0.6(10) . . . . ?
C10 N1 C9 C8 175.2(8) . . . . ?
C10 C15 C14 C13 0.8(11) . . . . ?
C12 C13 C14 C15 -1.9(11) . . . . ?
C14 C13 C12 C11 1.9(11) . . . . ?
C14 C15 C10 N1 178.9(6) . . . . ?
C14 C15 C10 C11 0.3(11) . . . . ?
C7 C8 C3 O3 -178.2(7) . . . . ?
C7 C8 C3 C4 2.4(11) . . . . ?
C7 C8 C9 N1 -178.4(7) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00104000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.808
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-17-HP-ESRF-8p72GPa
_database_code_depnum_ccdc_archive 'CCDC 2427941'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-17-HP-ESRF-8p72GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.439 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4602(7)
_cell_length_b                   14.0721(12)
_cell_length_c                   9.2088(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.068(8)
_cell_angle_gamma                90
_cell_volume                     1067.95(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    755
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.8720
_cell_measurement_theta_min      2.1140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.974
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0116
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.439
_diffrn_reflns_Laue_measured_fraction_max 0.374
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2308
_diffrn_reflns_point_group_measured_fraction_full 0.439
_diffrn_reflns_point_group_measured_fraction_max 0.374
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.789
_diffrn_reflns_theta_min         2.120
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.439
_diffrn_measured_fraction_theta_max 0.374
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291167000
_diffrn_orient_matrix_UB_12      0.0162021000
_diffrn_orient_matrix_UB_13      0.0200974000
_diffrn_orient_matrix_UB_21      0.0288979000
_diffrn_orient_matrix_UB_22      -0.0062422000
_diffrn_orient_matrix_UB_23      0.0409039000
_diffrn_orient_matrix_UB_31      0.0279646000
_diffrn_orient_matrix_UB_32      0.0233653000
_diffrn_orient_matrix_UB_33      -0.0029574000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1256
_reflns_number_total             1391
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1391
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+4.5162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0945
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47946(7) 0.45628(4) 0.63759(5) 0.0318(2) Uani 1 1 d D U . . .
Br1 Br 1.33657(9) 0.55391(5) 0.96904(7) 0.0330(3) Uani 1 1 d D U . . .
O3 O 0.2743(7) 0.5310(4) 0.5922(6) 0.0362(14) Uani 1 1 d D U . . .
N1 N 0.6091(7) 0.5745(4) 0.7305(6) 0.0290(11) Uani 1 1 d D U . . .
O2 O 0.2778(8) 0.2946(4) 0.4942(6) 0.046(2) Uani 1 1 d D U . . .
C8 C 0.3742(9) 0.6815(5) 0.6889(7) 0.0341(9) Uani 1 1 d D U . . .
C3 C 0.2509(9) 0.6203(5) 0.6128(7) 0.0341(10) Uani 1 1 d D U . . .
C9 C 0.5400(9) 0.6544(5) 0.7458(7) 0.0323(16) Uani 1 1 d D U . . .
H9 H 0.606369 0.700476 0.800994 0.039 Uiso 1 1 calc R U . . .
O1 O 0.7358(8) 0.3137(4) 0.7346(6) 0.048(2) Uani 1 1 d D U . . .
C13 C 1.1100(8) 0.5621(5) 0.8963(7) 0.0332(8) Uani 1 1 d D U . . .
C15 C 0.8744(8) 0.5134(5) 0.7203(7) 0.0329(8) Uani 1 1 d D U . . .
H15 H 0.824050 0.476260 0.639467 0.039 Uiso 1 1 calc R U . . .
C4 C 0.0956(9) 0.6583(5) 0.5588(7) 0.0349(10) Uani 1 1 d D U . . .
H4 H 0.012682 0.619438 0.507288 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7832(8) 0.5720(5) 0.7846(7) 0.0331(8) Uani 1 1 d D U . . .
C12 C 1.0232(8) 0.6218(5) 0.9620(7) 0.0336(8) Uani 1 1 d D U . . .
H12 H 1.074127 0.658547 1.043090 0.040 Uiso 1 1 calc R U . . .
C14 C 1.0414(8) 0.5074(5) 0.7723(7) 0.0331(8) Uani 1 1 d D U . . .
H14 H 1.104457 0.468624 0.726286 0.040 Uiso 1 1 calc R U . . .
C11 C 0.8552(8) 0.6279(5) 0.9064(7) 0.0337(8) Uani 1 1 d D U . . .
H11 H 0.792748 0.668557 0.950065 0.040 Uiso 1 1 calc R U . . .
C2 C 0.3537(10) 0.3527(5) 0.5488(8) 0.037(2) Uani 1 1 d D U . . .
C7 C 0.3391(9) 0.7758(5) 0.7113(7) 0.0350(10) Uani 1 1 d D U . . .
H7 H 0.420190 0.815287 0.764207 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6436(9) 0.3710(5) 0.6958(7) 0.0313(17) Uani 1 1 d D U . . .
C5 C 0.0647(9) 0.7517(5) 0.5809(7) 0.0357(10) Uani 1 1 d D U . . .
H5 H -0.039307 0.775514 0.544671 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1860(9) 0.8120(5) 0.6566(7) 0.0357(10) Uani 1 1 d D U . . .
H6 H 0.164051 0.875698 0.670008 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9078(12) 3_666 ?
Rh1 O3 1.991(5) . ?
Rh1 N1 2.069(5) . ?
Rh1 C2 1.879(6) . ?
Rh1 C1 1.821(6) . ?
Br1 C13 1.885(6) . ?
O3 C3 1.292(8) . ?
N1 C9 1.289(9) . ?
N1 C10 1.444(8) . ?
O2 C2 1.090(7) . ?
C8 C3 1.412(8) . ?
C8 C9 1.433(9) . ?
C8 C7 1.385(9) . ?
C3 C4 1.402(9) . ?
C9 H9 0.9300 . ?
O1 C1 1.123(8) . ?
C13 C12 1.347(11) . ?
C13 C14 1.390(8) . ?
C15 H15 0.9300 . ?
C15 C10 1.354(11) . ?
C15 C14 1.388(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.364(9) . ?
C10 C11 1.392(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.400(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.377(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(9) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.19(19) . 3_666 ?
O3 Rh1 N1 91.0(2) . . ?
N1 Rh1 Rh1 82.14(16) . 3_666 ?
C2 Rh1 Rh1 96.7(3) . 3_666 ?
C2 Rh1 O3 86.4(3) . . ?
C2 Rh1 N1 177.3(2) . . ?
C1 Rh1 Rh1 107.6(3) . 3_666 ?
C1 Rh1 O3 168.5(3) . . ?
C1 Rh1 N1 96.3(3) . . ?
C1 Rh1 C2 86.3(3) . . ?
C3 O3 Rh1 129.6(4) . . ?
C9 N1 Rh1 122.4(5) . . ?
C9 N1 C10 115.9(5) . . ?
C10 N1 Rh1 121.8(4) . . ?
C3 C8 C9 124.8(6) . . ?
C7 C8 C3 120.0(6) . . ?
C7 C8 C9 115.2(6) . . ?
O3 C3 C8 123.1(6) . . ?
O3 C3 C4 118.8(5) . . ?
C4 C3 C8 118.1(6) . . ?
N1 C9 C8 128.5(6) . . ?
N1 C9 H9 115.7 . . ?
C8 C9 H9 115.7 . . ?
C12 C13 Br1 119.5(4) . . ?
C12 C13 C14 123.0(6) . . ?
C14 C13 Br1 117.4(6) . . ?
C10 C15 H15 119.3 . . ?
C10 C15 C14 121.5(6) . . ?
C14 C15 H15 119.3 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(6) . . ?
C5 C4 H4 119.7 . . ?
C15 C10 N1 120.1(5) . . ?
C15 C10 C11 120.5(6) . . ?
C11 C10 N1 119.3(7) . . ?
C13 C12 H12 120.5 . . ?
C13 C12 C11 119.0(6) . . ?
C11 C12 H12 120.5 . . ?
C13 C14 H14 121.5 . . ?
C15 C14 C13 117.0(8) . . ?
C15 C14 H14 121.5 . . ?
C10 C11 C12 118.9(7) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
O2 C2 Rh1 177.7(6) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 C8 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
O1 C1 Rh1 174.4(8) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(6) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.0(6) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -6.5(12) . . . . ?
Rh1 O3 C3 C4 174.2(6) . . . . ?
Rh1 N1 C9 C8 -8.6(11) . . . . ?
Rh1 N1 C10 C15 30.5(10) . . . . ?
Rh1 N1 C10 C11 -147.3(5) . . . . ?
Br1 C13 C12 C11 179.5(5) . . . . ?
Br1 C13 C14 C15 179.5(5) . . . . ?
O3 C3 C4 C5 178.6(7) . . . . ?
N1 C10 C11 C12 177.3(6) . . . . ?
C8 C3 C4 C5 -0.7(12) . . . . ?
C8 C7 C6 C5 1.6(11) . . . . ?
C3 C8 C9 N1 5.3(14) . . . . ?
C3 C8 C7 C6 -2.0(12) . . . . ?
C3 C4 C5 C6 0.4(12) . . . . ?
C9 N1 C10 C15 -150.5(7) . . . . ?
C9 N1 C10 C11 31.7(9) . . . . ?
C9 C8 C3 O3 3.1(13) . . . . ?
C9 C8 C3 C4 -177.6(8) . . . . ?
C9 C8 C7 C6 177.2(7) . . . . ?
C13 C12 C11 C10 -0.1(9) . . . . ?
C15 C10 C11 C12 -0.5(10) . . . . ?
C4 C5 C6 C7 -0.8(11) . . . . ?
C10 N1 C9 C8 172.4(8) . . . . ?
C10 C15 C14 C13 2.0(12) . . . . ?
C12 C13 C14 C15 -2.7(12) . . . . ?
C14 C13 C12 C11 1.8(12) . . . . ?
C14 C15 C10 N1 -178.2(6) . . . . ?
C14 C15 C10 C11 -0.4(12) . . . . ?
C7 C8 C3 O3 -177.8(8) . . . . ?
C7 C8 C3 C4 1.5(12) . . . . ?
C7 C8 C9 N1 -173.9(8) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00372000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.698
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-03-HP-ESRF-0p50GPa
_database_code_depnum_ccdc_archive 'CCDC 2427932'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-03-HP-ESRF-0p50GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.453 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7978(8)
_cell_length_b                   15.0161(11)
_cell_length_c                   10.7766(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.709(8)
_cell_angle_gamma                90
_cell_volume                     1370.50(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    732
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.3990
_cell_measurement_theta_min      2.0090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.453
_diffrn_reflns_Laue_measured_fraction_max 0.389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3129
_diffrn_reflns_point_group_measured_fraction_full 0.453
_diffrn_reflns_point_group_measured_fraction_max 0.389
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.791
_diffrn_reflns_theta_min         1.930
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.453
_diffrn_measured_fraction_theta_max 0.389
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286739000
_diffrn_orient_matrix_UB_12      0.0152256000
_diffrn_orient_matrix_UB_13      -0.0157373000
_diffrn_orient_matrix_UB_21      -0.0251590000
_diffrn_orient_matrix_UB_22      -0.0077396000
_diffrn_orient_matrix_UB_23      -0.0361453000
_diffrn_orient_matrix_UB_31      -0.0296856000
_diffrn_orient_matrix_UB_32      0.0212611000
_diffrn_orient_matrix_UB_33      -0.0019376000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1502
_reflns_number_total             1851
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0485P)²+1.7383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1047
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48096(6) 0.46422(3) 0.64249(4) 0.03928(18) Uani 1 1 d D U . . .
Br1 Br 1.32342(8) 0.55758(5) 0.94866(6) 0.0519(3) Uani 1 1 d D U . . .
O3 O 0.2882(6) 0.5406(3) 0.5806(4) 0.0443(12) Uani 1 1 d D U . . .
N1 N 0.6118(6) 0.5759(3) 0.7217(4) 0.0389(10) Uani 1 1 d D U . . .
O2 O 0.2946(8) 0.3065(3) 0.5219(5) 0.067(2) Uani 1 1 d D U . . .
C8 C 0.3878(8) 0.6808(4) 0.6751(5) 0.0443(9) Uani 1 1 d D U . . .
C3 C 0.2672(8) 0.6242(4) 0.6027(5) 0.0441(9) Uani 1 1 d D U . . .
C9 C 0.5509(8) 0.6539(4) 0.7275(5) 0.0426(15) Uani 1 1 d D U . . .
H9 H 0.620000 0.697833 0.770290 0.051 Uiso 1 1 calc R U . . .
O1 O 0.7299(9) 0.3310(4) 0.7469(6) 0.083(3) Uani 1 1 d D U . . .
C13 C 1.1008(7) 0.5643(4) 0.8797(5) 0.0417(7) Uani 1 1 d D U . . .
C15 C 0.8713(8) 0.5277(4) 0.7124(5) 0.0416(7) Uani 1 1 d D U . . .
H15 H 0.823929 0.500022 0.634326 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1177(9) 0.6606(4) 0.5517(6) 0.0458(9) Uani 1 1 d D U . . .
H4 H 0.037792 0.625430 0.500825 0.055 Uiso 1 1 calc R U . . .
C10 C 0.7789(7) 0.5712(4) 0.7765(5) 0.0417(7) Uani 1 1 d D U . . .
C12 C 1.0127(7) 0.6071(4) 0.9456(5) 0.0424(7) Uani 1 1 d D U . . .
H12 H 1.060573 0.633771 1.024334 0.051 Uiso 1 1 calc R U . . .
C14 C 1.0348(8) 0.5239(4) 0.7616(5) 0.0418(7) Uani 1 1 d D U . . .
H14 H 1.097531 0.495235 0.716926 0.050 Uiso 1 1 calc R U . . .
C11 C 0.8497(7) 0.6109(4) 0.8949(5) 0.0424(7) Uani 1 1 d D U . . .
H11 H 0.788033 0.640040 0.940060 0.051 Uiso 1 1 calc R U . . .
C2 C 0.3611(9) 0.3651(4) 0.5665(5) 0.0463(19) Uani 1 1 d D U . . .
C7 C 0.3519(9) 0.7697(4) 0.6961(5) 0.0455(9) Uani 1 1 d D U . . .
H7 H 0.431293 0.806473 0.744164 0.055 Uiso 1 1 calc R U . . .
C1 C 0.6405(9) 0.3845(4) 0.7077(6) 0.0488(19) Uani 1 1 d D U . . .
C5 C 0.0867(9) 0.7473(4) 0.5754(5) 0.0468(9) Uani 1 1 d D U . . .
H5 H -0.015117 0.769314 0.542383 0.056 Uiso 1 1 calc R U . . .
C6 C 0.2036(8) 0.8037(4) 0.6477(5) 0.0467(9) Uani 1 1 d D U . . .
H6 H 0.181158 0.862606 0.662492 0.056 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 2.006(4) . ?
Rh1 N1 2.082(5) . ?
Rh1 C2 1.879(6) . ?
Rh1 C1 1.834(6) . ?
Br1 C13 1.900(6) . ?
O3 C3 1.301(7) . ?
N1 C9 1.297(7) . ?
N1 C10 1.430(7) . ?
O2 C2 1.093(7) . ?
C8 C3 1.417(8) . ?
C8 C9 1.450(8) . ?
C8 C7 1.404(8) . ?
C3 C4 1.392(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.124(7) . ?
C13 C12 1.347(9) . ?
C13 C14 1.388(7) . ?
C15 H15 0.9300 . ?
C15 C10 1.367(9) . ?
C15 C14 1.394(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.369(8) . ?
C10 C11 1.394(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.391(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.367(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 N1 89.98(19) . . ?
C2 Rh1 O3 89.1(2) . . ?
C2 Rh1 N1 178.4(2) . . ?
C1 Rh1 O3 172.4(3) . . ?
C1 Rh1 N1 95.0(2) . . ?
C1 Rh1 C2 86.0(3) . . ?
C3 O3 Rh1 129.8(3) . . ?
C9 N1 Rh1 123.9(4) . . ?
C9 N1 C10 114.6(5) . . ?
C10 N1 Rh1 121.5(4) . . ?
C3 C8 C9 124.2(5) . . ?
C7 C8 C3 119.4(5) . . ?
C7 C8 C9 116.4(5) . . ?
O3 C3 C8 123.9(5) . . ?
O3 C3 C4 118.1(5) . . ?
C4 C3 C8 118.0(5) . . ?
N1 C9 C8 127.7(5) . . ?
N1 C9 H9 116.2 . . ?
C8 C9 H9 116.2 . . ?
C12 C13 Br1 119.9(4) . . ?
C12 C13 C14 122.3(6) . . ?
C14 C13 Br1 117.8(5) . . ?
C10 C15 H15 119.3 . . ?
C10 C15 C14 121.4(5) . . ?
C14 C15 H15 119.3 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.9(5) . . ?
C5 C4 H4 119.5 . . ?
C15 C10 N1 120.0(5) . . ?
C15 C10 C11 119.2(5) . . ?
C11 C10 N1 120.8(6) . . ?
C13 C12 H12 120.3 . . ?
C13 C12 C11 119.5(5) . . ?
C11 C12 H12 120.3 . . ?
C13 C14 C15 117.6(7) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 H14 121.2 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0(6) . . ?
C12 C11 H11 120.0 . . ?
O2 C2 Rh1 178.2(8) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 C8 121.8(6) . . ?
C6 C7 H7 119.1 . . ?
O1 C1 Rh1 174.9(7) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(6) . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 118.1(6) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 3.0(10) . . . . ?
Rh1 O3 C3 C4 -177.3(5) . . . . ?
Rh1 N1 C9 C8 -4.2(10) . . . . ?
Rh1 N1 C10 C15 45.7(8) . . . . ?
Rh1 N1 C10 C11 -134.5(5) . . . . ?
Br1 C13 C12 C11 -179.4(4) . . . . ?
Br1 C13 C14 C15 178.9(5) . . . . ?
O3 C3 C4 C5 177.7(6) . . . . ?
N1 C10 C11 C12 -178.8(6) . . . . ?
C8 C3 C4 C5 -2.7(11) . . . . ?
C8 C7 C6 C5 -0.2(10) . . . . ?
C3 C8 C9 N1 -2.6(12) . . . . ?
C3 C8 C7 C6 -0.5(10) . . . . ?
C3 C4 C5 C6 2.0(11) . . . . ?
C9 N1 C10 C15 -135.1(7) . . . . ?
C9 N1 C10 C11 44.6(8) . . . . ?
C9 C8 C3 O3 3.4(11) . . . . ?
C9 C8 C3 C4 -176.2(7) . . . . ?
C9 C8 C7 C6 177.8(6) . . . . ?
C13 C12 C11 C10 -0.4(8) . . . . ?
C15 C10 C11 C12 0.9(8) . . . . ?
C4 C5 C6 C7 -0.5(9) . . . . ?
C10 N1 C9 C8 176.7(7) . . . . ?
C10 C15 C14 C13 1.3(10) . . . . ?
C12 C13 C14 C15 -0.8(10) . . . . ?
C14 C13 C12 C11 0.3(10) . . . . ?
C14 C15 C10 N1 178.3(6) . . . . ?
C14 C15 C10 C11 -1.4(10) . . . . ?
C7 C8 C3 O3 -178.5(6) . . . . ?
C7 C8 C3 C4 1.9(10) . . . . ?
C7 C8 C9 N1 179.3(6) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.03397000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.652
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-18-HP-ESRF-9p04GPa
_database_code_depnum_ccdc_archive 'CCDC 2427943'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-18-HP-ESRF-9p04GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.445 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4483(7)
_cell_length_b                   14.0668(11)
_cell_length_c                   9.1741(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.959(8)
_cell_angle_gamma                90
_cell_volume                     1062.50(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    701
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.8900
_cell_measurement_theta_min      2.1160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0131
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.445
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2333
_diffrn_reflns_point_group_measured_fraction_full 0.445
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.799
_diffrn_reflns_theta_min         2.123
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.445
_diffrn_measured_fraction_theta_max 0.379
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0291624000
_diffrn_orient_matrix_UB_12      0.0162882000
_diffrn_orient_matrix_UB_13      -0.0201531000
_diffrn_orient_matrix_UB_21      -0.0287667000
_diffrn_orient_matrix_UB_22      -0.0062824000
_diffrn_orient_matrix_UB_23      -0.0410359000
_diffrn_orient_matrix_UB_31      -0.0281282000
_diffrn_orient_matrix_UB_32      0.0233139000
_diffrn_orient_matrix_UB_33      0.0029347000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1276
_reflns_number_total             1404
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1404
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+5.3054P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0989
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47938(7) 0.45628(4) 0.63770(6) 0.0329(2) Uani 1 1 d D U . . .
Br1 Br 1.33680(9) 0.55379(5) 0.96934(8) 0.0342(3) Uani 1 1 d D U . . .
O3 O 0.2740(7) 0.5308(4) 0.5921(6) 0.0372(14) Uani 1 1 d D U . . .
N1 N 0.6088(8) 0.5748(4) 0.7302(6) 0.0321(13) Uani 1 1 d D U . . .
O2 O 0.2773(9) 0.2946(4) 0.4937(7) 0.048(2) Uani 1 1 d D U . . .
C8 C 0.3736(9) 0.6819(5) 0.6891(8) 0.0350(10) Uani 1 1 d D U . . .
C3 C 0.2503(9) 0.6201(5) 0.6129(8) 0.0349(10) Uani 1 1 d D U . . .
C9 C 0.5394(9) 0.6545(5) 0.7458(7) 0.0327(17) Uani 1 1 d D U . . .
H9 H 0.605842 0.700477 0.801286 0.039 Uiso 1 1 calc R U . . .
O1 O 0.7355(9) 0.3137(4) 0.7347(7) 0.051(2) Uani 1 1 d D U . . .
C13 C 1.1108(9) 0.5624(5) 0.8960(8) 0.0348(8) Uani 1 1 d D U . . .
C15 C 0.8748(9) 0.5133(5) 0.7210(8) 0.0347(8) Uani 1 1 d D U . . .
H15 H 0.824680 0.476443 0.639480 0.042 Uiso 1 1 calc R U . . .
C4 C 0.0941(10) 0.6583(5) 0.5591(8) 0.0357(10) Uani 1 1 d D U . . .
H4 H 0.010751 0.619386 0.508246 0.043 Uiso 1 1 calc R U . . .
C10 C 0.7827(9) 0.5718(5) 0.7854(8) 0.0349(8) Uani 1 1 d D U . . .
C12 C 1.0239(9) 0.6222(5) 0.9612(7) 0.0352(8) Uani 1 1 d D U . . .
H12 H 1.074892 0.659164 1.042259 0.042 Uiso 1 1 calc R U . . .
C14 C 1.0413(9) 0.5068(5) 0.7731(8) 0.0347(8) Uani 1 1 d D U . . .
H14 H 1.104000 0.466975 0.727837 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8556(9) 0.6284(5) 0.9061(7) 0.0353(8) Uani 1 1 d D U . . .
H11 H 0.793574 0.669759 0.949503 0.042 Uiso 1 1 calc R U . . .
C2 C 0.3540(11) 0.3525(5) 0.5491(9) 0.039(2) Uani 1 1 d D U . . .
C7 C 0.3382(10) 0.7763(5) 0.7112(8) 0.0357(10) Uani 1 1 d D U . . .
H7 H 0.419160 0.815899 0.764001 0.043 Uiso 1 1 calc R U . . .
C1 C 0.6436(10) 0.3708(5) 0.6962(8) 0.034(2) Uani 1 1 d D U . . .
C5 C 0.0641(10) 0.7517(5) 0.5809(8) 0.0365(10) Uani 1 1 d D U . . .
H5 H -0.039909 0.775489 0.544528 0.044 Uiso 1 1 calc R U . . .
C6 C 0.1850(9) 0.8123(5) 0.6560(7) 0.0364(10) Uani 1 1 d D U . . .
H6 H 0.162716 0.876099 0.668905 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9006(13) 3_666 ?
Rh1 O3 1.990(5) . ?
Rh1 N1 2.069(5) . ?
Rh1 C2 1.878(6) . ?
Rh1 C1 1.823(7) . ?
Br1 C13 1.881(7) . ?
O3 C3 1.293(8) . ?
N1 C9 1.287(9) . ?
N1 C10 1.443(8) . ?
O2 C2 1.093(8) . ?
C8 C3 1.415(9) . ?
C8 C9 1.433(9) . ?
C8 C7 1.386(10) . ?
C3 C4 1.408(9) . ?
C9 H9 0.9300 . ?
O1 C1 1.118(8) . ?
C13 C12 1.343(11) . ?
C13 C14 1.390(8) . ?
C15 H15 0.9300 . ?
C15 C10 1.356(11) . ?
C15 C14 1.383(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.361(10) . ?
C10 C11 1.391(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.401(9) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.376(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(9) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.1(2) . 3_666 ?
O3 Rh1 N1 91.0(2) . . ?
N1 Rh1 Rh1 81.95(19) . 3_666 ?
C2 Rh1 Rh1 96.8(3) . 3_666 ?
C2 Rh1 O3 86.4(3) . . ?
C2 Rh1 N1 177.3(3) . . ?
C1 Rh1 Rh1 107.7(3) . 3_666 ?
C1 Rh1 O3 168.3(4) . . ?
C1 Rh1 N1 96.5(3) . . ?
C1 Rh1 C2 86.2(3) . . ?
C3 O3 Rh1 129.6(4) . . ?
C9 N1 Rh1 122.3(5) . . ?
C9 N1 C10 116.1(6) . . ?
C10 N1 Rh1 121.5(5) . . ?
C3 C8 C9 124.4(6) . . ?
C7 C8 C3 120.1(6) . . ?
C7 C8 C9 115.5(6) . . ?
O3 C3 C8 123.3(6) . . ?
O3 C3 C4 118.9(6) . . ?
C4 C3 C8 117.9(6) . . ?
N1 C9 C8 128.8(6) . . ?
N1 C9 H9 115.6 . . ?
C8 C9 H9 115.6 . . ?
C12 C13 Br1 119.6(4) . . ?
C12 C13 C14 122.7(7) . . ?
C14 C13 Br1 117.7(6) . . ?
C10 C15 H15 119.1 . . ?
C10 C15 C14 121.9(6) . . ?
C14 C15 H15 119.1 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.5(6) . . ?
C5 C4 H4 119.8 . . ?
C15 C10 N1 120.3(6) . . ?
C15 C10 C11 120.0(7) . . ?
C11 C10 N1 119.8(7) . . ?
C13 C12 H12 120.3 . . ?
C13 C12 C11 119.4(6) . . ?
C11 C12 H12 120.3 . . ?
C13 C14 H14 121.5 . . ?
C15 C14 C13 117.1(8) . . ?
C15 C14 H14 121.5 . . ?
C10 C11 C12 119.0(8) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
O2 C2 Rh1 177.1(7) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 C8 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
O1 C1 Rh1 174.6(9) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.7(7) . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 118.8(7) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -6.2(13) . . . . ?
Rh1 O3 C3 C4 174.6(6) . . . . ?
Rh1 N1 C9 C8 -8.9(12) . . . . ?
Rh1 N1 C10 C15 31.3(10) . . . . ?
Rh1 N1 C10 C11 -148.0(5) . . . . ?
Br1 C13 C12 C11 180.0(5) . . . . ?
Br1 C13 C14 C15 179.5(6) . . . . ?
O3 C3 C4 C5 179.0(8) . . . . ?
N1 C10 C11 C12 177.9(7) . . . . ?
C8 C3 C4 C5 -0.2(13) . . . . ?
C8 C7 C6 C5 1.7(11) . . . . ?
C3 C8 C9 N1 5.4(15) . . . . ?
C3 C8 C7 C6 -1.9(12) . . . . ?
C3 C4 C5 C6 0.1(13) . . . . ?
C9 N1 C10 C15 -150.5(8) . . . . ?
C9 N1 C10 C11 30.2(10) . . . . ?
C9 C8 C3 O3 3.0(14) . . . . ?
C9 C8 C3 C4 -177.8(8) . . . . ?
C9 C8 C7 C6 177.1(8) . . . . ?
C13 C12 C11 C10 0.4(10) . . . . ?
C15 C10 C11 C12 -1.4(10) . . . . ?
C4 C5 C6 C7 -0.8(11) . . . . ?
C10 N1 C9 C8 172.9(8) . . . . ?
C10 C15 C14 C13 0.6(13) . . . . ?
C12 C13 C14 C15 -1.6(13) . . . . ?
C14 C13 C12 C11 1.1(13) . . . . ?
C14 C15 C10 N1 -178.4(7) . . . . ?
C14 C15 C10 C11 0.9(13) . . . . ?
C7 C8 C3 O3 -178.1(8) . . . . ?
C7 C8 C3 C4 1.2(13) . . . . ?
C7 C8 C9 N1 -173.6(8) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00372000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.815
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-02-HP-ESRF-0p28GPa
_database_code_depnum_ccdc_archive 'CCDC 2427931'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-02-HP-ESRF-0p28GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.454 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8362(8)
_cell_length_b                   15.1348(14)
_cell_length_c                   10.9325(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.932(9)
_cell_angle_gamma                90
_cell_volume                     1405.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    683
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.6430
_cell_measurement_theta_min      1.9040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.454
_diffrn_reflns_Laue_measured_fraction_max 0.385
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3129
_diffrn_reflns_point_group_measured_fraction_full 0.454
_diffrn_reflns_point_group_measured_fraction_max 0.385
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.791
_diffrn_reflns_theta_min         1.911
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.454
_diffrn_measured_fraction_theta_max 0.385
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0288123000
_diffrn_orient_matrix_UB_12      0.0150260000
_diffrn_orient_matrix_UB_13      0.0152597000
_diffrn_orient_matrix_UB_21      0.0249173000
_diffrn_orient_matrix_UB_22      -0.0076574000
_diffrn_orient_matrix_UB_23      0.0357759000
_diffrn_orient_matrix_UB_31      0.0294982000
_diffrn_orient_matrix_UB_32      0.0211614000
_diffrn_orient_matrix_UB_33      0.0021443000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1398
_reflns_number_total             1880
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1880
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+0.2848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1486
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48136(8) 0.46505(4) 0.64305(5) 0.0436(3) Uani 1 1 d D U . . .
Br1 Br 1.32200(10) 0.55787(6) 0.94666(7) 0.0580(3) Uani 1 1 d D U . . .
O3 O 0.2892(8) 0.5409(4) 0.5807(5) 0.0490(15) Uani 1 1 d D U . . .
N1 N 0.6125(8) 0.5766(4) 0.7197(5) 0.0409(11) Uani 1 1 d D U . . .
O2 O 0.2958(11) 0.3075(4) 0.5251(6) 0.073(3) Uani 1 1 d D U . . .
C8 C 0.3889(10) 0.6807(5) 0.6728(7) 0.0503(11) Uani 1 1 d D U . . .
C3 C 0.2695(10) 0.6242(5) 0.6017(6) 0.0501(11) Uani 1 1 d D U . . .
C9 C 0.5506(10) 0.6527(5) 0.7235(6) 0.0452(18) Uani 1 1 d D U . . .
H9 H 0.619812 0.696451 0.765006 0.054 Uiso 1 1 calc R U . . .
O1 O 0.7284(11) 0.3326(5) 0.7475(7) 0.088(3) Uani 1 1 d D U . . .
C13 C 1.1014(9) 0.5643(5) 0.8779(6) 0.0465(8) Uani 1 1 d D U . . .
C15 C 0.8710(10) 0.5290(5) 0.7110(6) 0.0463(9) Uani 1 1 d D U . . .
H15 H 0.823654 0.502191 0.633379 0.056 Uiso 1 1 calc R U . . .
C4 C 0.1199(11) 0.6612(5) 0.5508(7) 0.0513(11) Uani 1 1 d D U . . .
H4 H 0.040182 0.626429 0.500176 0.062 Uiso 1 1 calc R U . . .
C10 C 0.7789(9) 0.5716(5) 0.7752(6) 0.0465(9) Uani 1 1 d D U . . .
C12 C 1.0127(9) 0.6056(5) 0.9426(6) 0.0470(8) Uani 1 1 d D U . . .
H12 H 1.060182 0.631281 1.021044 0.056 Uiso 1 1 calc R U . . .
C14 C 1.0346(10) 0.5251(5) 0.7602(7) 0.0465(9) Uani 1 1 d D U . . .
H14 H 1.096832 0.497104 0.715679 0.056 Uiso 1 1 calc R U . . .
C11 C 0.8497(9) 0.6101(5) 0.8925(6) 0.0469(8) Uani 1 1 d D U . . .
H11 H 0.788559 0.638718 0.937308 0.056 Uiso 1 1 calc R U . . .
C2 C 0.3639(11) 0.3662(5) 0.5686(7) 0.052(2) Uani 1 1 d D U . . .
C7 C 0.3544(10) 0.7687(5) 0.6940(7) 0.0513(11) Uani 1 1 d D U . . .
H7 H 0.433555 0.805032 0.741956 0.062 Uiso 1 1 calc R U . . .
C1 C 0.6415(11) 0.3864(5) 0.7084(8) 0.053(2) Uani 1 1 d D U . . .
C5 C 0.0885(11) 0.7471(5) 0.5738(7) 0.0521(11) Uani 1 1 d D U . . .
H5 H -0.012905 0.769034 0.541126 0.062 Uiso 1 1 calc R U . . .
C6 C 0.2057(10) 0.8025(5) 0.6451(6) 0.0521(11) Uani 1 1 d D U . . .
H6 H 0.183798 0.861049 0.659434 0.062 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 2.007(5) . ?
Rh1 N1 2.089(6) . ?
Rh1 C2 1.874(7) . ?
Rh1 C1 1.837(7) . ?
Br1 C13 1.889(7) . ?
O3 C3 1.303(9) . ?
N1 C9 1.281(9) . ?
N1 C10 1.430(9) . ?
O2 C2 1.105(8) . ?
C8 C3 1.414(10) . ?
C8 C9 1.447(10) . ?
C8 C7 1.400(10) . ?
C3 C4 1.402(10) . ?
C9 H9 0.9300 . ?
O1 C1 1.120(9) . ?
C13 C12 1.346(11) . ?
C13 C14 1.393(8) . ?
C15 H15 0.9300 . ?
C15 C10 1.373(11) . ?
C15 C14 1.399(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(10) . ?
C10 C11 1.390(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.395(10) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.373(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(10) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 N1 89.9(2) . . ?
C2 Rh1 O3 89.6(3) . . ?
C2 Rh1 N1 178.0(3) . . ?
C1 Rh1 O3 172.7(4) . . ?
C1 Rh1 N1 94.8(3) . . ?
C1 Rh1 C2 85.8(4) . . ?
C3 O3 Rh1 129.5(5) . . ?
C9 N1 Rh1 123.1(5) . . ?
C9 N1 C10 115.6(6) . . ?
C10 N1 Rh1 121.4(5) . . ?
C3 C8 C9 122.9(7) . . ?
C7 C8 C3 120.2(7) . . ?
C7 C8 C9 116.9(7) . . ?
O3 C3 C8 124.5(7) . . ?
O3 C3 C4 118.3(7) . . ?
C4 C3 C8 117.2(7) . . ?
N1 C9 C8 129.5(7) . . ?
N1 C9 H9 115.2 . . ?
C8 C9 H9 115.2 . . ?
C12 C13 Br1 120.1(5) . . ?
C12 C13 C14 121.6(7) . . ?
C14 C13 Br1 118.4(7) . . ?
C10 C15 H15 119.4 . . ?
C10 C15 C14 121.2(6) . . ?
C14 C15 H15 119.4 . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.5(7) . . ?
C5 C4 H4 119.2 . . ?
C15 C10 N1 119.5(6) . . ?
C15 C10 C11 119.2(7) . . ?
C11 C10 N1 121.3(7) . . ?
C13 C12 H12 119.9 . . ?
C13 C12 C11 120.2(6) . . ?
C11 C12 H12 119.9 . . ?
C13 C14 C15 117.9(8) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C10 C11 C12 119.8(8) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 179.4(9) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 C8 121.2(7) . . ?
C6 C7 H7 119.4 . . ?
O1 C1 Rh1 173.4(9) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(7) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 118.6(7) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 2.6(13) . . . . ?
Rh1 O3 C3 C4 -177.4(6) . . . . ?
Rh1 N1 C9 C8 -4.2(12) . . . . ?
Rh1 N1 C10 C15 47.8(10) . . . . ?
Rh1 N1 C10 C11 -133.0(6) . . . . ?
Br1 C13 C12 C11 -179.6(5) . . . . ?
Br1 C13 C14 C15 179.0(6) . . . . ?
O3 C3 C4 C5 176.9(8) . . . . ?
N1 C10 C11 C12 -178.6(7) . . . . ?
C8 C3 C4 C5 -3.0(14) . . . . ?
C8 C7 C6 C5 0.2(11) . . . . ?
C3 C8 C9 N1 -3.1(15) . . . . ?
C3 C8 C7 C6 -1.0(13) . . . . ?
C3 C4 C5 C6 2.3(13) . . . . ?
C9 N1 C10 C15 -134.0(9) . . . . ?
C9 N1 C10 C11 45.2(10) . . . . ?
C9 C8 C3 O3 4.2(14) . . . . ?
C9 C8 C3 C4 -175.8(8) . . . . ?
C9 C8 C7 C6 177.3(8) . . . . ?
C13 C12 C11 C10 0.1(10) . . . . ?
C15 C10 C11 C12 0.6(10) . . . . ?
C4 C5 C6 C7 -0.8(11) . . . . ?
C10 N1 C9 C8 177.7(9) . . . . ?
C10 C15 C14 C13 1.3(13) . . . . ?
C12 C13 C14 C15 -0.6(13) . . . . ?
C14 C13 C12 C11 -0.1(12) . . . . ?
C14 C15 C10 N1 178.0(7) . . . . ?
C14 C15 C10 C11 -1.3(13) . . . . ?
C7 C8 C3 O3 -177.6(8) . . . . ?
C7 C8 C3 C4 2.3(13) . . . . ?
C7 C8 C9 N1 178.7(8) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.05668000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.625
_oxdiff_exptl_absorpt_empirical_full_min 0.464
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-16-HP-ESRF-8p05GPa
_database_code_depnum_ccdc_archive 'CCDC 2427939'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-16-HP-ESRF-8p05GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.442 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4750(6)
_cell_length_b                   14.0900(9)
_cell_length_c                   9.2705(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.248(6)
_cell_angle_gamma                90
_cell_volume                     1077.56(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    734
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.0780
_cell_measurement_theta_min      2.1070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.676
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.442
_diffrn_reflns_Laue_measured_fraction_max 0.377
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2362
_diffrn_reflns_point_group_measured_fraction_full 0.442
_diffrn_reflns_point_group_measured_fraction_max 0.377
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.795
_diffrn_reflns_theta_min         2.114
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.442
_diffrn_measured_fraction_theta_max 0.377
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293172000
_diffrn_orient_matrix_UB_12      0.0160366000
_diffrn_orient_matrix_UB_13      0.0198618000
_diffrn_orient_matrix_UB_21      0.0286990000
_diffrn_orient_matrix_UB_22      -0.0063434000
_diffrn_orient_matrix_UB_23      0.0407358000
_diffrn_orient_matrix_UB_31      0.0279134000
_diffrn_orient_matrix_UB_32      0.0233863000
_diffrn_orient_matrix_UB_33      -0.0025563000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1300
_reflns_number_total             1415
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1415
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0488P)²+6.1460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1187
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47960(8) 0.45647(4) 0.63740(6) 0.0284(2) Uani 1 1 d D U . . .
Br1 Br 1.33589(10) 0.55399(5) 0.96836(8) 0.0303(3) Uani 1 1 d D U . . .
O3 O 0.2756(8) 0.5317(4) 0.5910(6) 0.0329(15) Uani 1 1 d D U . . .
N1 N 0.6089(8) 0.5742(4) 0.7302(6) 0.0266(12) Uani 1 1 d D U . . .
O2 O 0.2781(10) 0.2946(5) 0.4947(7) 0.044(2) Uani 1 1 d D U . . .
C8 C 0.3751(10) 0.6812(5) 0.6890(8) 0.0306(10) Uani 1 1 d D U . . .
C3 C 0.2514(10) 0.6208(5) 0.6128(8) 0.0306(10) Uani 1 1 d D U . . .
C9 C 0.5402(10) 0.6541(5) 0.7462(8) 0.0285(18) Uani 1 1 d D U . . .
H9 H 0.606462 0.699735 0.802118 0.034 Uiso 1 1 calc R U . . .
O1 O 0.7349(10) 0.3140(5) 0.7346(7) 0.044(2) Uani 1 1 d D U . . .
C13 C 1.1103(10) 0.5629(5) 0.8953(8) 0.0304(8) Uani 1 1 d D U . . .
C15 C 0.8744(10) 0.5141(6) 0.7199(8) 0.0303(8) Uani 1 1 d D U . . .
H15 H 0.824436 0.478050 0.638140 0.036 Uiso 1 1 calc R U . . .
C4 C 0.0952(11) 0.6581(6) 0.5589(8) 0.0313(10) Uani 1 1 d D U . . .
H4 H 0.011870 0.619266 0.508463 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7821(10) 0.5719(6) 0.7853(8) 0.0305(8) Uani 1 1 d D U . . .
C12 C 1.0222(10) 0.6211(5) 0.9618(8) 0.0308(8) Uani 1 1 d D U . . .
H12 H 1.072680 0.657233 1.043302 0.037 Uiso 1 1 calc R U . . .
C14 C 1.0402(10) 0.5079(6) 0.7721(8) 0.0305(8) Uani 1 1 d D U . . .
H14 H 1.102759 0.468494 0.727056 0.037 Uiso 1 1 calc R U . . .
C11 C 0.8546(10) 0.6265(5) 0.9072(7) 0.0308(8) Uani 1 1 d D U . . .
H11 H 0.792219 0.666156 0.952039 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3547(12) 0.3530(6) 0.5493(9) 0.035(2) Uani 1 1 d D U . . .
C7 C 0.3382(11) 0.7757(5) 0.7126(8) 0.0313(10) Uani 1 1 d D U . . .
H7 H 0.418662 0.814840 0.766928 0.038 Uiso 1 1 calc R U . . .
C1 C 0.6440(11) 0.3716(6) 0.6960(8) 0.029(2) Uani 1 1 d D U . . .
C5 C 0.0669(11) 0.7515(6) 0.5813(8) 0.0320(11) Uani 1 1 d D U . . .
H5 H -0.036647 0.775577 0.544022 0.038 Uiso 1 1 calc R U . . .
C6 C 0.1864(10) 0.8123(6) 0.6576(8) 0.0320(11) Uani 1 1 d D U . . .
H6 H 0.164043 0.875895 0.670986 0.038 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9187(14) 3_666 ?
Rh1 O3 1.989(6) . ?
Rh1 N1 2.065(6) . ?
Rh1 C2 1.875(7) . ?
Rh1 C1 1.822(7) . ?
Br1 C13 1.881(7) . ?
O3 C3 1.296(9) . ?
N1 C9 1.291(10) . ?
N1 C10 1.439(9) . ?
O2 C2 1.097(9) . ?
C8 C3 1.409(9) . ?
C8 C9 1.430(10) . ?
C8 C7 1.396(10) . ?
C3 C4 1.405(10) . ?
C9 H9 0.9300 . ?
O1 C1 1.120(9) . ?
C13 C12 1.349(12) . ?
C13 C14 1.395(9) . ?
C15 H15 0.9300 . ?
C15 C10 1.364(12) . ?
C15 C14 1.380(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.363(10) . ?
C10 C11 1.388(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.397(10) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.372(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.390(10) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 81.8(2) . 3_666 ?
O3 Rh1 N1 90.8(2) . . ?
N1 Rh1 Rh1 82.41(19) . 3_666 ?
C2 Rh1 Rh1 96.6(3) . 3_666 ?
C2 Rh1 O3 86.8(3) . . ?
C2 Rh1 N1 177.5(3) . . ?
C1 Rh1 Rh1 107.5(3) . 3_666 ?
C1 Rh1 O3 169.0(4) . . ?
C1 Rh1 N1 96.1(3) . . ?
C1 Rh1 C2 86.4(4) . . ?
C3 O3 Rh1 130.1(5) . . ?
C9 N1 Rh1 122.5(5) . . ?
C9 N1 C10 115.4(6) . . ?
C10 N1 Rh1 122.0(5) . . ?
C3 C8 C9 125.2(7) . . ?
C7 C8 C3 119.1(7) . . ?
C7 C8 C9 115.6(6) . . ?
O3 C3 C8 122.5(7) . . ?
O3 C3 C4 118.5(6) . . ?
C4 C3 C8 119.0(7) . . ?
N1 C9 C8 128.3(7) . . ?
N1 C9 H9 115.9 . . ?
C8 C9 H9 115.9 . . ?
C12 C13 Br1 119.9(5) . . ?
C12 C13 C14 122.4(7) . . ?
C14 C13 Br1 117.7(7) . . ?
C10 C15 H15 119.2 . . ?
C10 C15 C14 121.6(7) . . ?
C14 C15 H15 119.2 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(7) . . ?
C5 C4 H4 120.3 . . ?
C15 C10 N1 119.8(6) . . ?
C15 C10 C11 120.0(7) . . ?
C11 C10 N1 120.1(8) . . ?
C13 C12 H12 120.3 . . ?
C13 C12 C11 119.4(6) . . ?
C11 C12 H12 120.3 . . ?
C13 C14 H14 121.3 . . ?
C15 C14 C13 117.4(8) . . ?
C15 C14 H14 121.3 . . ?
C10 C11 C12 119.2(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
O2 C2 Rh1 177.5(7) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.7(7) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 Rh1 173.7(9) . . ?
C4 C5 H5 118.7 . . ?
C4 C5 C6 122.7(7) . . ?
C6 C5 H5 118.7 . . ?
C7 C6 C5 118.0(7) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -5.2(14) . . . . ?
Rh1 O3 C3 C4 175.3(7) . . . . ?
Rh1 N1 C9 C8 -9.2(13) . . . . ?
Rh1 N1 C10 C15 31.8(11) . . . . ?
Rh1 N1 C10 C11 -146.5(6) . . . . ?
Br1 C13 C12 C11 -179.5(5) . . . . ?
Br1 C13 C14 C15 179.4(6) . . . . ?
O3 C3 C4 C5 179.6(9) . . . . ?
N1 C10 C11 C12 178.1(7) . . . . ?
C8 C3 C4 C5 0.1(14) . . . . ?
C8 C7 C6 C5 2.3(12) . . . . ?
C3 C8 C9 N1 5.7(16) . . . . ?
C3 C8 C7 C6 -3.0(13) . . . . ?
C3 C4 C5 C6 -0.9(14) . . . . ?
C9 N1 C10 C15 -149.9(9) . . . . ?
C9 N1 C10 C11 31.8(11) . . . . ?
C9 C8 C3 O3 2.3(15) . . . . ?
C9 C8 C3 C4 -178.2(9) . . . . ?
C9 C8 C7 C6 177.0(8) . . . . ?
C13 C12 C11 C10 -0.1(10) . . . . ?
C15 C10 C11 C12 -0.2(11) . . . . ?
C4 C5 C6 C7 -0.3(12) . . . . ?
C10 N1 C9 C8 172.5(9) . . . . ?
C10 C15 C14 C13 0.2(14) . . . . ?
C12 C13 C14 C15 -0.5(14) . . . . ?
C14 C13 C12 C11 0.5(13) . . . . ?
C14 C15 C10 N1 -178.1(8) . . . . ?
C14 C15 C10 C11 0.2(14) . . . . ?
C7 C8 C3 O3 -177.8(9) . . . . ?
C7 C8 C3 C4 1.8(14) . . . . ?
C7 C8 C9 N1 -174.2(9) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.03968000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.674
_oxdiff_exptl_absorpt_empirical_full_min 0.719
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-07-HP-ESRF-2p74GPa
_database_code_depnum_ccdc_archive 'CCDC 2427936'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-07-HP-ESRF-2p74GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.455 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7058(5)
_cell_length_b                   14.5531(7)
_cell_length_c                   10.0574(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.858(5)
_cell_angle_gamma                90
_cell_volume                     1231.64(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1086
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.6300
_cell_measurement_theta_min      2.0090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.455
_diffrn_reflns_Laue_measured_fraction_max 0.388
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2774
_diffrn_reflns_point_group_measured_fraction_full 0.455
_diffrn_reflns_point_group_measured_fraction_max 0.388
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.800
_diffrn_reflns_theta_min         2.015
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.455
_diffrn_measured_fraction_theta_max 0.388
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0285027000
_diffrn_orient_matrix_UB_12      0.0159096000
_diffrn_orient_matrix_UB_13      0.0171788000
_diffrn_orient_matrix_UB_21      0.0259986000
_diffrn_orient_matrix_UB_22      -0.0075702000
_diffrn_orient_matrix_UB_23      0.0384534000
_diffrn_orient_matrix_UB_31      0.0297443000
_diffrn_orient_matrix_UB_32      0.0219146000
_diffrn_orient_matrix_UB_33      0.0006549000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1494
_reflns_number_total             1661
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1661
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)²+2.1223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1033
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47947(6) 0.45996(3) 0.63938(4) 0.02488(16) Uani 1 1 d D U . . .
Br1 Br 1.32962(8) 0.55588(4) 0.95867(6) 0.0301(2) Uani 1 1 d D U . . .
O3 O 0.2806(6) 0.5366(3) 0.5850(4) 0.0298(11) Uani 1 1 d D U . . .
N1 N 0.6100(6) 0.5745(3) 0.7278(4) 0.0250(9) Uani 1 1 d D U . . .
O2 O 0.2904(7) 0.2990(3) 0.5051(5) 0.0449(17) Uani 1 1 d D U . . .
C8 C 0.3821(7) 0.6813(4) 0.6841(5) 0.0274(7) Uani 1 1 d D U . . .
C3 C 0.2607(8) 0.6229(4) 0.6087(5) 0.0277(7) Uani 1 1 d D U . . .
C9 C 0.5450(7) 0.6537(4) 0.7386(5) 0.0263(12) Uani 1 1 d D U . . .
H9 H 0.612614 0.698349 0.787845 0.032 Uiso 1 1 calc R U . . .
O1 O 0.7293(8) 0.3203(4) 0.7402(6) 0.0513(18) Uani 1 1 d D U . . .
C13 C 1.1062(7) 0.5635(4) 0.8877(5) 0.0263(6) Uani 1 1 d D U . . .
C15 C 0.8722(7) 0.5220(4) 0.7159(5) 0.0267(7) Uani 1 1 d D U . . .
H15 H 0.824035 0.492029 0.634182 0.032 Uiso 1 1 calc R U . . .
C4 C 0.1085(8) 0.6599(4) 0.5551(6) 0.0290(7) Uani 1 1 d D U . . .
H4 H 0.028336 0.623294 0.502035 0.035 Uiso 1 1 calc R U . . .
C10 C 0.7796(7) 0.5703(4) 0.7835(5) 0.0266(6) Uani 1 1 d D U . . .
C12 C 1.0170(7) 0.6134(4) 0.9569(5) 0.0267(6) Uani 1 1 d D U . . .
H12 H 1.066100 0.644351 1.037493 0.032 Uiso 1 1 calc R U . . .
C14 C 1.0366(7) 0.5170(4) 0.7667(5) 0.0268(6) Uani 1 1 d D U . . .
H14 H 1.098041 0.483466 0.720782 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8523(7) 0.6174(4) 0.9051(5) 0.0270(6) Uani 1 1 d D U . . .
H11 H 0.791014 0.651081 0.950990 0.032 Uiso 1 1 calc R U . . .
C2 C 0.3590(9) 0.3589(4) 0.5550(6) 0.0335(17) Uani 1 1 d D U . . .
C7 C 0.3453(8) 0.7730(4) 0.7072(5) 0.0283(7) Uani 1 1 d D U . . .
H7 H 0.424751 0.811172 0.757806 0.034 Uiso 1 1 calc R U . . .
C1 C 0.6409(8) 0.3770(4) 0.7013(6) 0.0306(15) Uani 1 1 d D U . . .
C5 C 0.0766(8) 0.7507(4) 0.5807(5) 0.0298(8) Uani 1 1 d D U . . .
H5 H -0.025426 0.773870 0.546415 0.036 Uiso 1 1 calc R U . . .
C6 C 0.1958(8) 0.8074(4) 0.6571(5) 0.0293(7) Uani 1 1 d D U . . .
H6 H 0.173714 0.868203 0.673863 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.1401(10) 3_666 ?
Rh1 O3 2.013(4) . ?
Rh1 N1 2.084(4) . ?
Rh1 C2 1.878(5) . ?
Rh1 C1 1.836(6) . ?
Br1 C13 1.895(6) . ?
O3 C3 1.298(7) . ?
N1 C9 1.300(7) . ?
N1 C10 1.440(7) . ?
O2 C2 1.102(7) . ?
C8 C3 1.415(7) . ?
C8 C9 1.441(8) . ?
C8 C7 1.406(8) . ?
C3 C4 1.404(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.127(7) . ?
C13 C12 1.375(9) . ?
C13 C14 1.389(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.374(9) . ?
C15 C14 1.392(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(8) . ?
C10 C11 1.403(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.396(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.364(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 80.72(16) . 3_666 ?
O3 Rh1 N1 90.55(18) . . ?
N1 Rh1 Rh1 84.83(14) . 3_666 ?
C2 Rh1 Rh1 93.8(2) . 3_666 ?
C2 Rh1 O3 88.3(2) . . ?
C2 Rh1 N1 178.28(19) . . ?
C1 Rh1 Rh1 107.1(2) . 3_666 ?
C1 Rh1 O3 170.5(3) . . ?
C1 Rh1 N1 95.5(2) . . ?
C1 Rh1 C2 85.9(3) . . ?
C3 O3 Rh1 129.2(4) . . ?
C9 N1 Rh1 122.9(4) . . ?
C9 N1 C10 115.5(5) . . ?
C10 N1 Rh1 121.6(4) . . ?
C3 C8 C9 124.3(5) . . ?
C7 C8 C3 119.2(5) . . ?
C7 C8 C9 116.5(5) . . ?
O3 C3 C8 124.3(5) . . ?
O3 C3 C4 117.3(5) . . ?
C4 C3 C8 118.5(5) . . ?
N1 C9 C8 128.5(5) . . ?
N1 C9 H9 115.7 . . ?
C8 C9 H9 115.7 . . ?
C12 C13 Br1 119.9(4) . . ?
C12 C13 C14 121.6(6) . . ?
C14 C13 Br1 118.5(5) . . ?
C10 C15 H15 119.2 . . ?
C10 C15 C14 121.6(5) . . ?
C14 C15 H15 119.2 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C15 C10 N1 120.2(4) . . ?
C15 C10 C11 119.3(5) . . ?
C11 C10 N1 120.4(6) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.5(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 C15 118.2(6) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.7(6) . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 178.9(8) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.5(5) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 Rh1 173.6(7) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(5) . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -1.6(10) . . . . ?
Rh1 O3 C3 C4 178.3(5) . . . . ?
Rh1 N1 C9 C8 -6.2(9) . . . . ?
Rh1 N1 C10 C15 40.6(7) . . . . ?
Rh1 N1 C10 C11 -141.2(4) . . . . ?
Br1 C13 C12 C11 -178.9(4) . . . . ?
Br1 C13 C14 C15 179.3(4) . . . . ?
O3 C3 C4 C5 177.5(6) . . . . ?
N1 C10 C11 C12 -179.2(5) . . . . ?
C8 C3 C4 C5 -2.6(10) . . . . ?
C8 C7 C6 C5 -0.3(9) . . . . ?
C3 C8 C9 N1 1.2(11) . . . . ?
C3 C8 C7 C6 -0.8(9) . . . . ?
C3 C4 C5 C6 1.6(10) . . . . ?
C9 N1 C10 C15 -140.3(6) . . . . ?
C9 N1 C10 C11 37.8(8) . . . . ?
C9 C8 C3 O3 3.2(11) . . . . ?
C9 C8 C3 C4 -176.7(6) . . . . ?
C9 C8 C7 C6 178.2(6) . . . . ?
C13 C12 C11 C10 0.2(8) . . . . ?
C15 C10 C11 C12 -1.1(8) . . . . ?
C4 C5 C6 C7 0.0(9) . . . . ?
C10 N1 C9 C8 174.8(6) . . . . ?
C10 C15 C14 C13 -1.0(10) . . . . ?
C12 C13 C14 C15 0.0(9) . . . . ?
C14 C13 C12 C11 0.4(9) . . . . ?
C14 C15 C10 N1 179.7(5) . . . . ?
C14 C15 C10 C11 1.5(9) . . . . ?
C7 C8 C3 O3 -177.9(6) . . . . ?
C7 C8 C3 C4 2.3(9) . . . . ?
C7 C8 C9 N1 -177.7(6) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.01999000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.714
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-14-HP-ESRF-6p82GPa
_database_code_depnum_ccdc_archive 'CCDC 2427938'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-14-HP-ESRF-6p82GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.450 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5105(4)
_cell_length_b                   14.1436(8)
_cell_length_c                   9.3971(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.615(5)
_cell_angle_gamma                90
_cell_volume                     1099.33(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    926
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.0620
_cell_measurement_theta_min      2.0920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.623
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.450
_diffrn_reflns_Laue_measured_fraction_max 0.381
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2433
_diffrn_reflns_point_group_measured_fraction_full 0.450
_diffrn_reflns_point_group_measured_fraction_max 0.381
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.797
_diffrn_reflns_theta_min         2.099
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.450
_diffrn_measured_fraction_theta_max 0.381
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0285908000
_diffrn_orient_matrix_UB_12      0.0163809000
_diffrn_orient_matrix_UB_13      -0.0195548000
_diffrn_orient_matrix_UB_21      -0.0280726000
_diffrn_orient_matrix_UB_22      -0.0069487000
_diffrn_orient_matrix_UB_23      -0.0403113000
_diffrn_orient_matrix_UB_31      -0.0290685000
_diffrn_orient_matrix_UB_32      0.0228314000
_diffrn_orient_matrix_UB_33      0.0017555000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1335
_reflns_number_total             1457
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1457
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0632P)²+5.8232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1366
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47963(9) 0.45689(4) 0.63737(6) 0.0246(3) Uani 1 1 d D U . . .
Br1 Br 1.33480(11) 0.55427(6) 0.96686(8) 0.0270(3) Uani 1 1 d D U . . .
O3 O 0.2754(9) 0.5325(4) 0.5914(6) 0.0296(16) Uani 1 1 d D U . . .
N1 N 0.6087(9) 0.5744(5) 0.7304(7) 0.0232(12) Uani 1 1 d D U . . .
O2 O 0.2805(11) 0.2953(5) 0.4954(8) 0.040(2) Uani 1 1 d D U . . .
C8 C 0.3762(11) 0.6817(6) 0.6883(9) 0.0271(10) Uani 1 1 d D U . . .
C3 C 0.2526(11) 0.6211(6) 0.6124(9) 0.0268(10) Uani 1 1 d D U . . .
C9 C 0.5402(10) 0.6534(6) 0.7458(8) 0.0256(18) Uani 1 1 d D U . . .
H9 H 0.606418 0.698500 0.802321 0.031 Uiso 1 1 calc R U . . .
O1 O 0.7334(11) 0.3141(5) 0.7349(8) 0.043(3) Uani 1 1 d D U . . .
C13 C 1.1102(10) 0.5635(6) 0.8936(8) 0.0257(8) Uani 1 1 d D U . . .
C15 C 0.8730(10) 0.5156(6) 0.7191(8) 0.0259(8) Uani 1 1 d D U . . .
H15 H 0.823245 0.480677 0.636933 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0975(11) 0.6587(6) 0.5589(9) 0.0275(11) Uani 1 1 d D U . . .
H4 H 0.014790 0.620249 0.507441 0.033 Uiso 1 1 calc R U . . .
C10 C 0.7815(10) 0.5717(6) 0.7862(8) 0.0259(8) Uani 1 1 d D U . . .
C12 C 1.0201(10) 0.6190(5) 0.9622(8) 0.0262(8) Uani 1 1 d D U . . .
H12 H 1.069649 0.653282 1.045101 0.031 Uiso 1 1 calc R U . . .
C14 C 1.0386(10) 0.5099(6) 0.7717(8) 0.0258(8) Uani 1 1 d D U . . .
H14 H 1.100626 0.471090 0.726574 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8541(10) 0.6243(5) 0.9076(7) 0.0262(8) Uani 1 1 d D U . . .
H11 H 0.791942 0.663092 0.952640 0.031 Uiso 1 1 calc R U . . .
C2 C 0.3545(12) 0.3533(6) 0.5502(9) 0.030(2) Uani 1 1 d D U . . .
C7 C 0.3396(11) 0.7759(6) 0.7118(8) 0.0277(11) Uani 1 1 d D U . . .
H7 H 0.420175 0.814989 0.765157 0.033 Uiso 1 1 calc R U . . .
C1 C 0.6426(11) 0.3719(6) 0.6963(9) 0.027(2) Uani 1 1 d D U . . .
C5 C 0.0677(11) 0.7516(6) 0.5820(8) 0.0283(11) Uani 1 1 d D U . . .
H5 H -0.035925 0.775440 0.545979 0.034 Uiso 1 1 calc R U . . .
C6 C 0.1885(11) 0.8118(6) 0.6584(8) 0.0284(11) Uani 1 1 d D U . . .
H6 H 0.166325 0.875001 0.672571 0.034 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9484(14) 3_666 ?
Rh1 O3 2.000(6) . ?
Rh1 N1 2.069(6) . ?
Rh1 C2 1.882(7) . ?
Rh1 C1 1.820(8) . ?
Br1 C13 1.878(8) . ?
O3 C3 1.290(9) . ?
N1 C9 1.285(10) . ?
N1 C10 1.440(10) . ?
O2 C2 1.087(9) . ?
C8 C3 1.413(10) . ?
C8 C9 1.430(10) . ?
C8 C7 1.397(11) . ?
C3 C4 1.402(11) . ?
C9 H9 0.9300 . ?
O1 C1 1.125(9) . ?
C13 C12 1.361(12) . ?
C13 C14 1.389(9) . ?
C15 H15 0.9300 . ?
C15 C10 1.367(12) . ?
C15 C14 1.381(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.366(11) . ?
C10 C11 1.380(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.388(10) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.364(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(10) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.2(2) . 3_666 ?
O3 Rh1 N1 90.5(3) . . ?
N1 Rh1 Rh1 82.96(19) . 3_666 ?
C2 Rh1 Rh1 96.4(3) . 3_666 ?
C2 Rh1 O3 87.0(3) . . ?
C2 Rh1 N1 177.6(3) . . ?
C1 Rh1 Rh1 107.5(3) . 3_666 ?
C1 Rh1 O3 168.6(4) . . ?
C1 Rh1 N1 96.4(3) . . ?
C1 Rh1 C2 86.1(4) . . ?
C3 O3 Rh1 129.9(5) . . ?
C9 N1 Rh1 122.4(6) . . ?
C9 N1 C10 115.7(6) . . ?
C10 N1 Rh1 121.8(5) . . ?
C3 C8 C9 124.5(7) . . ?
C7 C8 C3 119.4(7) . . ?
C7 C8 C9 116.2(7) . . ?
O3 C3 C8 123.0(7) . . ?
O3 C3 C4 118.4(7) . . ?
C4 C3 C8 118.6(7) . . ?
N1 C9 C8 129.0(7) . . ?
N1 C9 H9 115.5 . . ?
C8 C9 H9 115.5 . . ?
C12 C13 Br1 120.3(5) . . ?
C12 C13 C14 121.3(7) . . ?
C14 C13 Br1 118.4(7) . . ?
C10 C15 H15 119.6 . . ?
C10 C15 C14 120.9(7) . . ?
C14 C15 H15 119.6 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(7) . . ?
C5 C4 H4 119.9 . . ?
C15 C10 N1 119.4(6) . . ?
C15 C10 C11 120.1(7) . . ?
C11 C10 N1 120.5(8) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.6(7) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.4(8) . . ?
C15 C14 H14 120.8 . . ?
C10 C11 C12 119.7(8) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 177.5(8) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.5(7) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 173.9(10) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(8) . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 118.6(8) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -5.9(14) . . . . ?
Rh1 O3 C3 C4 174.8(7) . . . . ?
Rh1 N1 C9 C8 -9.7(13) . . . . ?
Rh1 N1 C10 C15 33.5(11) . . . . ?
Rh1 N1 C10 C11 -145.6(6) . . . . ?
Br1 C13 C12 C11 -179.3(5) . . . . ?
Br1 C13 C14 C15 179.0(7) . . . . ?
O3 C3 C4 C5 178.4(9) . . . . ?
N1 C10 C11 C12 178.4(7) . . . . ?
C8 C3 C4 C5 -0.9(15) . . . . ?
C8 C7 C6 C5 1.7(12) . . . . ?
C3 C8 C9 N1 6.6(16) . . . . ?
C3 C8 C7 C6 -2.5(13) . . . . ?
C3 C4 C5 C6 0.1(14) . . . . ?
C9 N1 C10 C15 -148.4(9) . . . . ?
C9 N1 C10 C11 32.5(11) . . . . ?
C9 C8 C3 O3 2.1(16) . . . . ?
C9 C8 C3 C4 -178.6(9) . . . . ?
C9 C8 C7 C6 178.1(9) . . . . ?
C13 C12 C11 C10 1.3(10) . . . . ?
C15 C10 C11 C12 -0.7(11) . . . . ?
C4 C5 C6 C7 -0.5(12) . . . . ?
C10 N1 C9 C8 172.2(9) . . . . ?
C10 C15 C14 C13 -0.7(14) . . . . ?
C12 C13 C14 C15 1.3(14) . . . . ?
C14 C13 C12 C11 -1.6(13) . . . . ?
C14 C15 C10 N1 -178.7(8) . . . . ?
C14 C15 C10 C11 0.4(14) . . . . ?
C7 C8 C3 O3 -177.2(9) . . . . ?
C7 C8 C3 C4 2.1(14) . . . . ?
C7 C8 C9 N1 -174.1(9) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.02356000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.387
_oxdiff_exptl_absorpt_empirical_full_min 0.695
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-1p54GPa
_database_code_depnum_ccdc_archive 'CCDC 2427951'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-1p54GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.464 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7611(5)
_cell_length_b                   14.727(7)
_cell_length_c                   10.3538(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.283(6)
_cell_angle_gamma                90
_cell_volume                     1288.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1754
_cell_measurement_theta_min      2.4450
_cell_measurement_theta_max      28.5210

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.434
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.747
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_T_max  0.328
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3594
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.464
_diffrn_reflns_theta_max         25.335
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.464
_diffrn_measured_fraction_theta_full 0.464
_diffrn_reflns_Laue_measured_fraction_max 0.464
_diffrn_reflns_Laue_measured_fraction_full 0.464
_diffrn_reflns_point_group_measured_fraction_max 0.464
_diffrn_reflns_point_group_measured_fraction_full 0.464
_reflns_number_total             1098
_reflns_number_gt                927
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+6.1215P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1098
_refine_ls_number_parameters     184
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47983(6) 0.46120(9) 0.64066(5) 0.0218(5) Uani 1 1 d D U . . .
Br1 Br 1.32723(8) 0.55688(12) 0.95483(7) 0.0262(8) Uani 1 1 d D U . . .
O3 O 0.2836(5) 0.5384(7) 0.5834(5) 0.0265(11) Uani 1 1 d D U . . .
N1 N 0.6109(6) 0.5746(8) 0.7257(5) 0.0202(11) Uani 1 1 d D U . . .
O2 O 0.2931(7) 0.3016(8) 0.5113(6) 0.038(3) Uani 1 1 d D U . . .
C8 C 0.3839(8) 0.6813(9) 0.6803(7) 0.0242(8) Uani 1 1 d D U . . .
O1 O 0.7282(7) 0.3242(9) 0.7439(6) 0.052(4) Uani 1 1 d D U . . .
C9 C 0.5482(8) 0.6530(10) 0.7348(6) 0.0221(15) Uani 1 1 d D U . . .
H9 H 0.616493 0.697037 0.782091 0.027 Uiso 1 1 calc R U . . .
C3 C 0.2650(8) 0.6231(9) 0.6058(7) 0.0242(8) Uani 1 1 d D U . . .
C10 C 0.7797(7) 0.5711(9) 0.7823(6) 0.0201(7) Uani 1 1 d D U . . .
C15 C 0.8722(7) 0.5234(10) 0.7141(6) 0.0201(7) Uani 1 1 d D U . . .
H15 H 0.824540 0.493771 0.634301 0.024 Uiso 1 1 calc R U . . .
C13 C 1.1044(7) 0.5639(9) 0.8837(6) 0.0199(7) Uani 1 1 d D U . . .
C11 C 0.8521(7) 0.6153(8) 0.9015(6) 0.0201(7) Uani 1 1 d D U . . .
H11 H 0.790911 0.647472 0.946877 0.024 Uiso 1 1 calc R U . . .
C14 C 1.0347(7) 0.5202(10) 0.7651(6) 0.0200(7) Uani 1 1 d D U . . .
H14 H 1.096653 0.488813 0.719679 0.024 Uiso 1 1 calc R U . . .
C12 C 1.0150(7) 0.6117(8) 0.9529(6) 0.0203(7) Uani 1 1 d D U . . .
H12 H 1.063501 0.640929 1.032762 0.024 Uiso 1 1 calc R U . . .
C7 C 0.3492(8) 0.7705(9) 0.7032(7) 0.0249(8) Uani 1 1 d D U . . .
H7 H 0.429105 0.807446 0.753376 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1110(8) 0.6599(10) 0.5548(7) 0.0250(8) Uani 1 1 d D U . . .
H4 H 0.029746 0.624063 0.504071 0.030 Uiso 1 1 calc R U . . .
C2 C 0.3590(8) 0.3621(10) 0.5603(7) 0.0243(11) Uani 1 1 d D U . . .
C1 C 0.6390(8) 0.3776(10) 0.7044(7) 0.0243(11) Uani 1 1 d D U . . .
C5 C 0.0836(9) 0.7478(9) 0.5805(7) 0.0256(8) Uani 1 1 d D U . . .
H5 H -0.018329 0.770468 0.547486 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2003(8) 0.8061(9) 0.6539(6) 0.0255(8) Uani 1 1 d D U . . .
H6 H 0.178139 0.866342 0.668768 0.031 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.847(11) . ?
Rh1 C2 1.865(12) . ?
Rh1 O3 2.015(7) . ?
Rh1 N1 2.086(9) . ?
Br1 C13 1.899(6) . ?
O3 C3 1.288(14) . ?
N1 C9 1.292(14) . ?
N1 C10 1.441(8) . ?
O2 C2 1.109(13) . ?
C8 C7 1.382(14) . ?
C8 C3 1.411(12) . ?
C8 C9 1.461(10) . ?
O1 C1 1.107(13) . ?
C9 H9 0.9300 . ?
C3 C4 1.420(11) . ?
C10 C11 1.392(10) . ?
C10 C15 1.397(11) . ?
C15 C14 1.383(8) . ?
C15 H15 0.9300 . ?
C13 C14 1.378(11) . ?
C13 C12 1.385(11) . ?
C11 C12 1.386(8) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.374(10) . ?
C7 H7 0.9300 . ?
C4 C5 1.355(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(12) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 85.7(5) . . ?
C1 Rh1 O3 170.5(4) . . ?
C2 Rh1 O3 88.3(4) . . ?
C1 Rh1 N1 95.9(4) . . ?
C2 Rh1 N1 178.2(4) . . ?
O3 Rh1 N1 90.3(3) . . ?
C3 O3 Rh1 129.2(5) . . ?
C9 N1 C10 114.4(9) . . ?
C9 N1 Rh1 123.3(5) . . ?
C10 N1 Rh1 122.3(8) . . ?
C7 C8 C3 120.4(8) . . ?
C7 C8 C9 116.4(9) . . ?
C3 C8 C9 123.2(11) . . ?
N1 C9 C8 128.4(10) . . ?
N1 C9 H9 115.8 . . ?
C8 C9 H9 115.8 . . ?
O3 C3 C8 125.2(8) . . ?
O3 C3 C4 117.1(9) . . ?
C8 C3 C4 117.6(11) . . ?
C11 C10 C15 119.6(6) . . ?
C11 C10 N1 121.5(7) . . ?
C15 C10 N1 118.9(7) . . ?
C14 C15 C10 120.0(8) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
C14 C13 C12 121.3(6) . . ?
C14 C13 Br1 119.3(6) . . ?
C12 C13 Br1 119.4(6) . . ?
C12 C11 C10 120.3(7) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C14 C15 119.7(8) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C13 C12 C11 119.1(7) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C6 C7 C8 122.0(9) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C5 C4 C3 119.4(10) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
O2 C2 Rh1 176.8(8) . . ?
O1 C1 Rh1 176.0(10) . . ?
C4 C5 C6 123.5(9) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C7 C6 C5 117.1(11) . . ?
C7 C6 H6 121.5 . . ?
C5 C6 H6 121.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 175.5(7) . . . . ?
Rh1 N1 C9 C8 -5.9(12) . . . . ?
C7 C8 C9 N1 -178.9(8) . . . . ?
C3 C8 C9 N1 -0.1(13) . . . . ?
Rh1 O3 C3 C8 -1.0(13) . . . . ?
Rh1 O3 C3 C4 -179.0(5) . . . . ?
C7 C8 C3 O3 -177.2(8) . . . . ?
C9 C8 C3 O3 4.1(13) . . . . ?
C7 C8 C3 C4 0.8(12) . . . . ?
C9 C8 C3 C4 -178.0(7) . . . . ?
C9 N1 C10 C11 40.0(12) . . . . ?
Rh1 N1 C10 C11 -138.7(8) . . . . ?
C9 N1 C10 C15 -138.9(10) . . . . ?
Rh1 N1 C10 C15 42.5(11) . . . . ?
C11 C10 C15 C14 0.1(16) . . . . ?
N1 C10 C15 C14 178.9(12) . . . . ?
C15 C10 C11 C12 -0.4(12) . . . . ?
N1 C10 C11 C12 -179.2(10) . . . . ?
C12 C13 C14 C15 -0.4(17) . . . . ?
Br1 C13 C14 C15 178.6(10) . . . . ?
C10 C15 C14 C13 0.3(18) . . . . ?
C14 C13 C12 C11 0.1(15) . . . . ?
Br1 C13 C12 C11 -179.0(7) . . . . ?
C10 C11 C12 C13 0.3(11) . . . . ?
C3 C8 C7 C6 -0.7(12) . . . . ?
C9 C8 C7 C6 178.1(6) . . . . ?
O3 C3 C4 C5 177.2(8) . . . . ?
C8 C3 C4 C5 -0.9(12) . . . . ?
C3 C4 C5 C6 1.1(12) . . . . ?
C8 C7 C6 C5 0.8(10) . . . . ?
C4 C5 C6 C7 -1.0(10) . . . . ?

_refine_diff_density_max         0.464
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.090



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-08-HP-ESRF-3p18GPa
_database_code_depnum_ccdc_archive 'CCDC 2427944'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-08-HP-ESRF-3p18GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.444 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6910(7)
_cell_length_b                   14.4947(8)
_cell_length_c                   9.9702(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.738(6)
_cell_angle_gamma                90
_cell_volume                     1214.66(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    845
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.7830
_cell_measurement_theta_min      2.0210
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.444
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2676
_diffrn_reflns_point_group_measured_fraction_full 0.444
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.790
_diffrn_reflns_theta_min         2.026
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.444
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0292049000
_diffrn_orient_matrix_UB_12      0.0156939000
_diffrn_orient_matrix_UB_13      0.0170203000
_diffrn_orient_matrix_UB_21      0.0252524000
_diffrn_orient_matrix_UB_22      -0.0078526000
_diffrn_orient_matrix_UB_23      0.0388822000
_diffrn_orient_matrix_UB_31      0.0297886000
_diffrn_orient_matrix_UB_32      0.0221184000
_diffrn_orient_matrix_UB_33      0.0015615000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1441
_reflns_number_total             1610
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1610
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0667P)²+0.8537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1053
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47950(6) 0.45949(3) 0.63900(4) 0.02427(17) Uani 1 1 d D U . . .
Br1 Br 1.33029(8) 0.55566(4) 0.95999(6) 0.0292(2) Uani 1 1 d D U . . .
O3 O 0.2803(6) 0.5360(3) 0.5861(4) 0.0299(11) Uani 1 1 d D U . . .
N1 N 0.6098(6) 0.5744(3) 0.7282(4) 0.0246(9) Uani 1 1 d D U . . .
O2 O 0.2886(7) 0.2977(3) 0.5035(5) 0.0421(16) Uani 1 1 d D U . . .
C8 C 0.3810(8) 0.6820(4) 0.6852(5) 0.0268(7) Uani 1 1 d D U . . .
C3 C 0.2608(8) 0.6226(4) 0.6095(5) 0.0269(7) Uani 1 1 d D U . . .
C9 C 0.5437(7) 0.6533(4) 0.7398(5) 0.0251(12) Uani 1 1 d D U . . .
H9 H 0.611146 0.697835 0.790587 0.030 Uiso 1 1 calc R U . . .
O1 O 0.7285(8) 0.3187(4) 0.7395(6) 0.0513(19) Uani 1 1 d D U . . .
C13 C 1.1060(7) 0.5641(4) 0.8889(5) 0.0255(6) Uani 1 1 d D U . . .
C15 C 0.8731(7) 0.5213(4) 0.7165(5) 0.0257(7) Uani 1 1 d D U . . .
H15 H 0.825038 0.490752 0.634537 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1077(8) 0.6607(4) 0.5560(6) 0.0281(7) Uani 1 1 d D U . . .
H4 H 0.027576 0.624005 0.502202 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7796(7) 0.5704(4) 0.7841(5) 0.0257(6) Uani 1 1 d D U . . .
C12 C 1.0178(7) 0.6143(4) 0.9577(5) 0.0260(6) Uani 1 1 d D U . . .
H12 H 1.067234 0.645455 1.038794 0.031 Uiso 1 1 calc R U . . .
C14 C 1.0374(7) 0.5163(4) 0.7674(5) 0.0260(6) Uani 1 1 d D U . . .
H14 H 1.099284 0.482167 0.721800 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8532(7) 0.6187(4) 0.9062(5) 0.0263(6) Uani 1 1 d D U . . .
H11 H 0.792206 0.653288 0.952057 0.032 Uiso 1 1 calc R U . . .
C2 C 0.3574(9) 0.3583(4) 0.5536(6) 0.0351(18) Uani 1 1 d D U . . .
C7 C 0.3453(8) 0.7741(4) 0.7085(5) 0.0277(7) Uani 1 1 d D U . . .
H7 H 0.424920 0.812418 0.759104 0.033 Uiso 1 1 calc R U . . .
C1 C 0.6407(8) 0.3763(4) 0.7006(6) 0.0291(14) Uani 1 1 d D U . . .
C5 C 0.0747(8) 0.7502(4) 0.5815(5) 0.0290(7) Uani 1 1 d D U . . .
H5 H -0.028016 0.772948 0.548209 0.035 Uiso 1 1 calc R U . . .
C6 C 0.1954(8) 0.8082(4) 0.6579(5) 0.0288(7) Uani 1 1 d D U . . .
H6 H 0.173135 0.869423 0.673770 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.1130(10) 3_666 ?
Rh1 O3 2.010(4) . ?
Rh1 N1 2.082(4) . ?
Rh1 C2 1.882(5) . ?
Rh1 C1 1.831(6) . ?
Br1 C13 1.901(6) . ?
O3 C3 1.296(7) . ?
N1 C9 1.299(7) . ?
N1 C10 1.440(7) . ?
O2 C2 1.107(7) . ?
C8 C3 1.414(7) . ?
C8 C9 1.441(8) . ?
C8 C7 1.403(8) . ?
C3 C4 1.414(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.131(7) . ?
C13 C12 1.362(9) . ?
C13 C14 1.392(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.378(9) . ?
C15 C14 1.390(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(8) . ?
C10 C11 1.409(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.393(8) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.365(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.407(8) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 81.05(16) . 3_666 ?
O3 Rh1 N1 90.54(18) . . ?
N1 Rh1 Rh1 84.59(14) . 3_666 ?
C2 Rh1 Rh1 94.0(2) . 3_666 ?
C2 Rh1 O3 87.8(2) . . ?
C2 Rh1 N1 178.02(19) . . ?
C1 Rh1 Rh1 107.2(2) . 3_666 ?
C1 Rh1 O3 170.1(3) . . ?
C1 Rh1 N1 95.5(2) . . ?
C1 Rh1 C2 86.2(3) . . ?
C3 O3 Rh1 129.1(4) . . ?
C9 N1 Rh1 122.5(4) . . ?
C9 N1 C10 115.7(5) . . ?
C10 N1 Rh1 121.7(4) . . ?
C3 C8 C9 123.1(5) . . ?
C7 C8 C3 120.2(5) . . ?
C7 C8 C9 116.7(5) . . ?
O3 C3 C8 125.0(5) . . ?
O3 C3 C4 117.6(5) . . ?
C4 C3 C8 117.4(5) . . ?
N1 C9 C8 129.4(5) . . ?
N1 C9 H9 115.3 . . ?
C8 C9 H9 115.3 . . ?
C12 C13 Br1 120.1(4) . . ?
C12 C13 C14 122.2(6) . . ?
C14 C13 Br1 117.7(5) . . ?
C10 C15 H15 119.1 . . ?
C10 C15 C14 121.8(5) . . ?
C14 C15 H15 119.1 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.5(5) . . ?
C5 C4 H4 119.3 . . ?
C15 C10 N1 120.4(4) . . ?
C15 C10 C11 119.0(5) . . ?
C11 C10 N1 120.6(6) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.7(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 H14 121.2 . . ?
C15 C14 C13 117.7(6) . . ?
C15 C14 H14 121.2 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(6) . . ?
C12 C11 H11 120.2 . . ?
O2 C2 Rh1 178.4(7) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 C8 121.0(5) . . ?
C6 C7 H7 119.5 . . ?
O1 C1 Rh1 173.0(7) . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.6(5) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -2.7(10) . . . . ?
Rh1 O3 C3 C4 177.7(5) . . . . ?
Rh1 N1 C9 C8 -7.1(9) . . . . ?
Rh1 N1 C10 C15 39.9(8) . . . . ?
Rh1 N1 C10 C11 -142.0(4) . . . . ?
Br1 C13 C12 C11 -178.8(4) . . . . ?
Br1 C13 C14 C15 179.0(4) . . . . ?
O3 C3 C4 C5 176.8(6) . . . . ?
N1 C10 C11 C12 -179.6(5) . . . . ?
C8 C3 C4 C5 -2.9(10) . . . . ?
C8 C7 C6 C5 0.1(9) . . . . ?
C3 C8 C9 N1 2.2(11) . . . . ?
C3 C8 C7 C6 -0.6(9) . . . . ?
C3 C4 C5 C6 2.5(10) . . . . ?
C9 N1 C10 C15 -141.4(6) . . . . ?
C9 N1 C10 C11 36.7(8) . . . . ?
C9 C8 C3 O3 3.4(11) . . . . ?
C9 C8 C3 C4 -177.0(6) . . . . ?
C9 C8 C7 C6 178.4(6) . . . . ?
C13 C12 C11 C10 0.7(8) . . . . ?
C15 C10 C11 C12 -1.5(8) . . . . ?
C4 C5 C6 C7 -1.1(9) . . . . ?
C10 N1 C9 C8 174.3(6) . . . . ?
C10 C15 C14 C13 -1.1(10) . . . . ?
C12 C13 C14 C15 0.3(9) . . . . ?
C14 C13 C12 C11 -0.1(9) . . . . ?
C14 C15 C10 N1 179.8(5) . . . . ?
C14 C15 C10 C11 1.7(9) . . . . ?
C7 C8 C3 O3 -177.8(6) . . . . ?
C7 C8 C3 C4 1.9(9) . . . . ?
C7 C8 C9 N1 -176.8(6) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00372000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.643
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-2p68GPa
_database_code_depnum_ccdc_archive 'CCDC 2427954'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-2p68GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.376 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-0p00GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.467 Why?
RESPONSE: ...
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.696(5)
_cell_length_b                   14.544(2)
_cell_length_c                   10.092(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.80(8)
_cell_angle_gamma                90
_cell_volume                     1228.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1338
_cell_measurement_theta_min      2.7950
_cell_measurement_theta_max      28.0410

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.653
_shelx_estimated_absorpt_T_min   0.653
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_T_max  0.340
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3290
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.522
_diffrn_reflns_theta_max         25.312
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.374
_diffrn_measured_fraction_theta_full 0.376
_diffrn_reflns_Laue_measured_fraction_max 0.374
_diffrn_reflns_Laue_measured_fraction_full 0.376
_diffrn_reflns_point_group_measured_fraction_max 0.374
_diffrn_reflns_point_group_measured_fraction_full 0.376
_reflns_number_total             839
_reflns_number_gt                690
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+4.8725P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         839
_refine_ls_number_parameters     190
_refine_ls_number_restraints     266
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47900(17) 0.46059(5) 0.64032(17) 0.0262(13) Uani 1 1 d D U . . .
Br1 Br 1.3302(2) 0.55555(7) 0.9581(2) 0.0278(12) Uani 1 1 d D U . . .
O3 O 0.2792(13) 0.5358(4) 0.5889(13) 0.0198(11) Uani 1 1 d D U . . .
N1 N 0.6077(14) 0.5744(5) 0.7319(15) 0.016(3) Uani 1 1 d D U . . .
O2 O 0.2904(15) 0.3005(5) 0.5054(15) 0.042(12) Uani 1 1 d D U . . .
C8 C 0.3835(16) 0.6811(6) 0.6821(18) 0.0217(9) Uani 1 1 d D U . . .
O1 O 0.7284(15) 0.3216(5) 0.7385(15) 0.038(12) Uani 1 1 d D U . . .
C9 C 0.5450(18) 0.6535(6) 0.7376(19) 0.0208(12) Uani 1 1 d D U . . .
H9 H 0.614312 0.698780 0.784230 0.025 Uiso 1 1 calc R U . . .
C3 C 0.2628(17) 0.6235(6) 0.6077(18) 0.0217(9) Uani 1 1 d D U . . .
C10 C 0.7788(14) 0.5709(6) 0.7845(14) 0.0168(9) Uani 1 1 d D U . . .
C15 C 0.8699(15) 0.5209(6) 0.7189(15) 0.0166(9) Uani 1 1 d D U . . .
H15 H 0.819912 0.490266 0.637747 0.020 Uiso 1 1 calc R U . . .
C13 C 1.1053(14) 0.5635(6) 0.8875(14) 0.0161(9) Uani 1 1 d D U . . .
C11 C 0.8542(14) 0.6177(5) 0.9030(13) 0.0168(9) Uani 1 1 d D U . . .
H11 H 0.793543 0.652143 0.947959 0.020 Uiso 1 1 calc R U . . .
C14 C 1.0336(15) 0.5150(6) 0.7700(15) 0.0165(9) Uani 1 1 d D U . . .
H14 H 1.093747 0.479162 0.726354 0.020 Uiso 1 1 calc R U . . .
C12 C 1.0174(14) 0.6147(6) 0.9562(14) 0.0166(9) Uani 1 1 d D U . . .
H12 H 1.067433 0.646295 1.036431 0.020 Uiso 1 1 calc R U . . .
C7 C 0.3477(17) 0.7734(6) 0.7053(17) 0.0220(9) Uani 1 1 d D U . . .
H7 H 0.428093 0.811853 0.755301 0.026 Uiso 1 1 calc R U . . .
C4 C 0.1084(18) 0.6603(6) 0.5555(19) 0.0220(9) Uani 1 1 d D U . . .
H4 H 0.026487 0.623512 0.503576 0.026 Uiso 1 1 calc R U . . .
C2 C 0.360(2) 0.3606(6) 0.556(2) 0.024(6) Uani 1 1 d D U . . .
C1 C 0.6393(18) 0.3782(6) 0.700(2) 0.022(5) Uani 1 1 d D U . . .
C5 C 0.0785(18) 0.7499(6) 0.5808(18) 0.0223(9) Uani 1 1 d D U . . .
H5 H -0.024388 0.773224 0.547022 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1981(16) 0.8062(6) 0.6556(17) 0.0223(9) Uani 1 1 d D U . . .
H6 H 0.175642 0.867072 0.671801 0.027 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.813(10) . ?
Rh1 C2 1.853(8) . ?
Rh1 O3 1.998(9) . ?
Rh1 N1 2.070(7) . ?
Rh1 Rh1 3.167(5) 3_666 ?
Br1 C13 1.893(11) . ?
O3 C3 1.304(10) . ?
N1 C9 1.280(13) . ?
N1 C10 1.437(14) . ?
O2 C2 1.104(9) . ?
C8 C3 1.392(11) . ?
C8 C7 1.411(13) . ?
C8 C9 1.421(14) . ?
O1 C1 1.124(10) . ?
C9 H9 0.9300 . ?
C3 C4 1.407(14) . ?
C10 C15 1.371(17) . ?
C10 C11 1.377(13) . ?
C15 C14 1.378(14) . ?
C15 H15 0.9300 . ?
C13 C14 1.374(13) . ?
C13 C12 1.381(17) . ?
C11 C12 1.374(13) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.348(13) . ?
C7 H7 0.9300 . ?
C4 C5 1.367(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(12) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 85.2(5) . . ?
C1 Rh1 O3 169.6(8) . . ?
C2 Rh1 O3 88.5(5) . . ?
C1 Rh1 N1 96.1(4) . . ?
C2 Rh1 N1 178.6(4) . . ?
O3 Rh1 N1 90.3(3) . . ?
C1 Rh1 Rh1 105.8(9) . 3_666 ?
C2 Rh1 Rh1 93.3(8) . 3_666 ?
O3 Rh1 Rh1 82.7(5) . 3_666 ?
N1 Rh1 Rh1 86.0(5) . 3_666 ?
C3 O3 Rh1 128.3(7) . . ?
C9 N1 C10 115.2(8) . . ?
C9 N1 Rh1 123.6(8) . . ?
C10 N1 Rh1 121.0(7) . . ?
C3 C8 C7 119.5(10) . . ?
C3 C8 C9 124.2(10) . . ?
C7 C8 C9 116.3(8) . . ?
N1 C9 C8 128.6(9) . . ?
N1 C9 H9 115.7 . . ?
C8 C9 H9 115.7 . . ?
O3 C3 C8 124.8(9) . . ?
O3 C3 C4 116.6(8) . . ?
C8 C3 C4 118.4(9) . . ?
C15 C10 C11 118.7(10) . . ?
C15 C10 N1 121.1(10) . . ?
C11 C10 N1 120.2(13) . . ?
C10 C15 C14 121.8(11) . . ?
C10 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C14 C13 C12 121.8(11) . . ?
C14 C13 Br1 118.2(11) . . ?
C12 C13 Br1 120.0(7) . . ?
C12 C11 C10 121.3(12) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C14 C15 118.1(13) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C11 C12 C13 118.4(10) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C6 C7 C8 120.7(9) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C5 C4 C3 120.2(9) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
O2 C2 Rh1 179.4(18) . . ?
O1 C1 Rh1 173.7(16) . . ?
C4 C5 C6 121.1(10) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 120.1(10) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 173(2) . . . . ?
Rh1 N1 C9 C8 -2(3) . . . . ?
C3 C8 C9 N1 -1(4) . . . . ?
C7 C8 C9 N1 180(2) . . . . ?
Rh1 O3 C3 C8 -7(3) . . . . ?
Rh1 O3 C3 C4 177.1(15) . . . . ?
C7 C8 C3 O3 -175(2) . . . . ?
C9 C8 C3 O3 6(3) . . . . ?
C7 C8 C3 C4 1(3) . . . . ?
C9 C8 C3 C4 -178(2) . . . . ?
C9 N1 C10 C15 -139.2(16) . . . . ?
Rh1 N1 C10 C15 36.2(18) . . . . ?
C9 N1 C10 C11 41(2) . . . . ?
Rh1 N1 C10 C11 -143.6(10) . . . . ?
C11 C10 C15 C14 1.4(17) . . . . ?
N1 C10 C15 C14 -178.3(12) . . . . ?
C15 C10 C11 C12 -0.4(13) . . . . ?
N1 C10 C11 C12 179.3(11) . . . . ?
C12 C13 C14 C15 2.1(18) . . . . ?
Br1 C13 C14 C15 -180.0(10) . . . . ?
C10 C15 C14 C13 -2.2(19) . . . . ?
C10 C11 C12 C13 0.3(12) . . . . ?
C14 C13 C12 C11 -1.1(16) . . . . ?
Br1 C13 C12 C11 -179.0(7) . . . . ?
C3 C8 C7 C6 0(3) . . . . ?
C9 C8 C7 C6 179.4(17) . . . . ?
O3 C3 C4 C5 175(2) . . . . ?
C8 C3 C4 C5 -2(3) . . . . ?
C3 C4 C5 C6 1(3) . . . . ?
C8 C7 C6 C5 -0.3(18) . . . . ?
C4 C5 C6 C7 0.0(19) . . . . ?

_refine_diff_density_max         0.446
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.098



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-2p06GPa
_database_code_depnum_ccdc_archive 'CCDC 2427953'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-2p06GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.466 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6680(5)
_cell_length_b                   14.816(6)
_cell_length_c                   10.1546(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.305(7)
_cell_angle_gamma                90
_cell_volume                     1257.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1701
_cell_measurement_theta_min      2.4590
_cell_measurement_theta_max      29.1520

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.543
_shelx_estimated_absorpt_T_min   0.635
_shelx_estimated_absorpt_T_max   0.742
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_T_max  0.326
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3291
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.493
_diffrn_reflns_theta_max         25.331
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.465
_diffrn_measured_fraction_theta_full 0.466
_diffrn_reflns_Laue_measured_fraction_max 0.465
_diffrn_reflns_Laue_measured_fraction_full 0.466
_diffrn_reflns_point_group_measured_fraction_max 0.465
_diffrn_reflns_point_group_measured_fraction_full 0.466
_reflns_number_total             1071
_reflns_number_gt                861
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²+6.0073P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1071
_refine_ls_number_parameters     184
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48002(8) 0.46030(10) 0.63991(6) 0.0222(6) Uani 1 1 d D U . . .
Br1 Br 1.32764(10) 0.55692(14) 0.95684(8) 0.0252(9) Uani 1 1 d D U . . .
O3 O 0.2834(7) 0.5357(8) 0.5851(6) 0.0249(13) Uani 1 1 d D U . . .
N1 N 0.6118(8) 0.5746(9) 0.7261(6) 0.0203(13) Uani 1 1 d D U . . .
O2 O 0.2911(8) 0.3011(10) 0.5080(7) 0.042(3) Uani 1 1 d D U . . .
C8 C 0.3836(9) 0.6817(10) 0.6829(8) 0.0226(9) Uani 1 1 d D U . . .
O1 O 0.7289(9) 0.3235(10) 0.7431(8) 0.054(4) Uani 1 1 d D U . . .
C9 C 0.5492(10) 0.6532(11) 0.7385(8) 0.0232(18) Uani 1 1 d D U . . .
H9 H 0.618405 0.696238 0.788682 0.028 Uiso 1 1 calc R U . . .
C3 C 0.2642(10) 0.6203(10) 0.6083(8) 0.0228(9) Uani 1 1 d D U . . .
C10 C 0.7799(9) 0.5694(10) 0.7833(7) 0.0182(7) Uani 1 1 d D U . . .
C15 C 0.8717(9) 0.5213(11) 0.7148(8) 0.0182(8) Uani 1 1 d D U . . .
H15 H 0.822746 0.490603 0.634759 0.022 Uiso 1 1 calc R U . . .
C13 C 1.1050(9) 0.5636(11) 0.8855(8) 0.0180(7) Uani 1 1 d D U . . .
C11 C 0.8528(9) 0.6142(9) 0.9039(7) 0.0183(8) Uani 1 1 d D U . . .
H11 H 0.790779 0.646278 0.949795 0.022 Uiso 1 1 calc R U . . .
C14 C 1.0353(9) 0.5188(11) 0.7651(7) 0.0182(8) Uani 1 1 d D U . . .
H14 H 1.097991 0.487598 0.718811 0.022 Uiso 1 1 calc R U . . .
C12 C 1.0167(9) 0.6113(9) 0.9558(7) 0.0184(8) Uani 1 1 d D U . . .
H12 H 1.066177 0.640974 1.036610 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3465(10) 0.7731(10) 0.7054(8) 0.0231(9) Uani 1 1 d D U . . .
H7 H 0.427342 0.810069 0.755952 0.028 Uiso 1 1 calc R U . . .
C4 C 0.1103(10) 0.6591(11) 0.5555(8) 0.0233(9) Uani 1 1 d D U . . .
H4 H 0.027980 0.624157 0.502476 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3572(10) 0.3605(10) 0.5572(9) 0.0233(13) Uani 1 1 d D U . . .
C1 C 0.6403(11) 0.3772(11) 0.7037(8) 0.0233(13) Uani 1 1 d D U . . .
C5 C 0.0815(11) 0.7480(10) 0.5818(8) 0.0236(9) Uani 1 1 d D U . . .
H5 H -0.022125 0.769758 0.548337 0.028 Uiso 1 1 calc R U . . .
C6 C 0.1989(9) 0.8081(10) 0.6562(7) 0.0234(9) Uani 1 1 d D U . . .
H6 H 0.175877 0.868101 0.670427 0.028 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.841(12) . ?
Rh1 C2 1.884(12) . ?
Rh1 O3 1.990(8) . ?
Rh1 N1 2.101(11) . ?
Rh1 Rh1 3.1777(17) 3_666 ?
Br1 C13 1.877(8) . ?
O3 C3 1.294(15) . ?
N1 C9 1.304(15) . ?
N1 C10 1.421(9) . ?
O2 C2 1.096(14) . ?
C8 C7 1.424(15) . ?
C8 C3 1.435(13) . ?
C8 C9 1.459(11) . ?
O1 C1 1.105(14) . ?
C9 H9 0.9300 . ?
C3 C4 1.421(12) . ?
C10 C15 1.386(12) . ?
C10 C11 1.389(11) . ?
C15 C14 1.375(10) . ?
C15 H15 0.9300 . ?
C13 C12 1.373(12) . ?
C13 C14 1.382(12) . ?
C11 C12 1.379(10) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.349(12) . ?
C7 H7 0.9300 . ?
C4 C5 1.380(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.412(13) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 85.3(6) . . ?
C1 Rh1 O3 169.9(5) . . ?
C2 Rh1 O3 88.5(5) . . ?
C1 Rh1 N1 96.6(5) . . ?
C2 Rh1 N1 177.8(5) . . ?
O3 Rh1 N1 89.7(4) . . ?
C1 Rh1 Rh1 108.2(3) . 3_666 ?
C2 Rh1 Rh1 94.2(3) . 3_666 ?
O3 Rh1 Rh1 80.2(2) . 3_666 ?
N1 Rh1 Rh1 84.2(2) . 3_666 ?
C3 O3 Rh1 129.4(7) . . ?
C9 N1 C10 114.6(10) . . ?
C9 N1 Rh1 124.5(6) . . ?
C10 N1 Rh1 120.8(9) . . ?
C7 C8 C3 121.7(9) . . ?
C7 C8 C9 116.9(10) . . ?
C3 C8 C9 121.3(12) . . ?
N1 C9 C8 127.8(12) . . ?
N1 C9 H9 116.1 . . ?
C8 C9 H9 116.1 . . ?
O3 C3 C4 118.5(10) . . ?
O3 C3 C8 126.9(9) . . ?
C4 C3 C8 114.6(11) . . ?
C15 C10 C11 120.0(8) . . ?
C15 C10 N1 119.1(8) . . ?
C11 C10 N1 120.9(8) . . ?
C14 C15 C10 120.0(9) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
C12 C13 C14 122.3(8) . . ?
C12 C13 Br1 118.9(6) . . ?
C14 C13 Br1 118.8(7) . . ?
C12 C11 C10 120.4(8) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C15 C14 C13 118.9(9) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.6 . . ?
C13 C12 C11 118.5(8) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C6 C7 C8 122.6(11) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C5 C4 C3 120.9(11) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
O2 C2 Rh1 177.2(10) . . ?
O1 C1 Rh1 175.3(12) . . ?
C4 C5 C6 124.3(10) . . ?
C4 C5 H5 117.8 . . ?
C6 C5 H5 117.8 . . ?
C7 C6 C5 115.7(12) . . ?
C7 C6 H6 122.1 . . ?
C5 C6 H6 122.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 175.5(8) . . . . ?
Rh1 N1 C9 C8 -7.9(14) . . . . ?
C7 C8 C9 N1 -177.1(9) . . . . ?
C3 C8 C9 N1 2.5(15) . . . . ?
Rh1 O3 C3 C4 178.9(6) . . . . ?
Rh1 O3 C3 C8 -0.8(15) . . . . ?
C7 C8 C3 O3 -178.0(9) . . . . ?
C9 C8 C3 O3 2.4(15) . . . . ?
C7 C8 C3 C4 2.3(13) . . . . ?
C9 C8 C3 C4 -177.3(8) . . . . ?
C9 N1 C10 C15 -140.6(11) . . . . ?
Rh1 N1 C10 C15 42.6(13) . . . . ?
C9 N1 C10 C11 37.3(13) . . . . ?
Rh1 N1 C10 C11 -139.5(9) . . . . ?
C11 C10 C15 C14 -0.9(18) . . . . ?
N1 C10 C15 C14 177.0(13) . . . . ?
C15 C10 C11 C12 0.2(13) . . . . ?
N1 C10 C11 C12 -177.7(12) . . . . ?
C10 C15 C14 C13 1(2) . . . . ?
C12 C13 C14 C15 -1(2) . . . . ?
Br1 C13 C14 C15 178.0(11) . . . . ?
C14 C13 C12 C11 0.1(17) . . . . ?
Br1 C13 C12 C11 -178.7(8) . . . . ?
C10 C11 C12 C13 0.2(12) . . . . ?
C3 C8 C7 C6 -1.4(13) . . . . ?
C9 C8 C7 C6 178.3(7) . . . . ?
O3 C3 C4 C5 177.4(9) . . . . ?
C8 C3 C4 C5 -2.9(13) . . . . ?
C3 C4 C5 C6 2.6(14) . . . . ?
C8 C7 C6 C5 0.8(11) . . . . ?
C4 C5 C6 C7 -1.4(11) . . . . ?

_refine_diff_density_max         0.508
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.110



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-13-HP-ESRF-6p14GPa
_database_code_depnum_ccdc_archive 'CCDC 2427946'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-13-HP-ESRF-6p14GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.452 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5393(4)
_cell_length_b                   14.1915(7)
_cell_length_c                   9.4827(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.837(4)
_cell_angle_gamma                90
_cell_volume                     1115.82(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1092
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.0080
_cell_measurement_theta_min      2.0810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.452
_diffrn_reflns_Laue_measured_fraction_max 0.383
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2477
_diffrn_reflns_point_group_measured_fraction_full 0.452
_diffrn_reflns_point_group_measured_fraction_max 0.383
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.796
_diffrn_reflns_theta_min         2.088
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.383
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0284035000
_diffrn_orient_matrix_UB_12      0.0163667000
_diffrn_orient_matrix_UB_13      0.0193205000
_diffrn_orient_matrix_UB_21      0.0275629000
_diffrn_orient_matrix_UB_22      -0.0073318000
_diffrn_orient_matrix_UB_23      0.0400448000
_diffrn_orient_matrix_UB_31      0.0295454000
_diffrn_orient_matrix_UB_32      0.0225941000
_diffrn_orient_matrix_UB_33      -0.0010195000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1370
_reflns_number_total             1487
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1487
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+2.7325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0895
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47949(6) 0.45718(3) 0.63752(4) 0.02621(16) Uani 1 1 d D U . . .
Br1 Br 1.33421(7) 0.55453(4) 0.96586(5) 0.02883(19) Uani 1 1 d D U . . .
O3 O 0.2762(6) 0.5326(3) 0.5911(4) 0.0307(10) Uani 1 1 d D U . . .
N1 N 0.6093(6) 0.5743(3) 0.7302(4) 0.0253(9) Uani 1 1 d D U . . .
O2 O 0.2822(7) 0.2954(3) 0.4967(5) 0.0431(16) Uani 1 1 d D U . . .
C8 C 0.3772(7) 0.6818(4) 0.6882(5) 0.0279(8) Uani 1 1 d D U . . .
C3 C 0.2546(7) 0.6216(4) 0.6119(5) 0.0280(8) Uani 1 1 d D U . . .
C9 C 0.5414(7) 0.6537(4) 0.7449(5) 0.0268(12) Uani 1 1 d D U . . .
H9 H 0.608097 0.698871 0.799874 0.032 Uiso 1 1 calc R U . . .
O1 O 0.7321(7) 0.3146(3) 0.7351(5) 0.0439(16) Uani 1 1 d D U . . .
C13 C 1.1092(7) 0.5625(4) 0.8934(5) 0.0272(6) Uani 1 1 d D U . . .
C15 C 0.8726(7) 0.5165(4) 0.7191(5) 0.0273(6) Uani 1 1 d D U . . .
H15 H 0.822952 0.482087 0.637107 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1000(8) 0.6593(4) 0.5590(6) 0.0295(8) Uani 1 1 d D U . . .
H4 H 0.017538 0.621006 0.507694 0.035 Uiso 1 1 calc R U . . .
C10 C 0.7812(7) 0.5711(4) 0.7857(5) 0.0273(6) Uani 1 1 d D U . . .
C12 C 1.0214(7) 0.6186(4) 0.9609(5) 0.0278(6) Uani 1 1 d D U . . .
H12 H 1.071880 0.653196 1.042326 0.033 Uiso 1 1 calc R U . . .
C14 C 1.0387(7) 0.5111(4) 0.7709(5) 0.0272(6) Uani 1 1 d D U . . .
H14 H 1.100836 0.473877 0.724603 0.033 Uiso 1 1 calc R U . . .
C11 C 0.8549(7) 0.6240(4) 0.9075(5) 0.0280(6) Uani 1 1 d D U . . .
H11 H 0.793430 0.662462 0.952604 0.034 Uiso 1 1 calc R U . . .
C2 C 0.3549(8) 0.3543(4) 0.5504(6) 0.0311(15) Uani 1 1 d D U . . .
C7 C 0.3411(8) 0.7762(4) 0.7115(5) 0.0291(8) Uani 1 1 d D U . . .
H7 H 0.421660 0.815300 0.763869 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6419(8) 0.3728(4) 0.6966(6) 0.0312(14) Uani 1 1 d D U . . .
C5 C 0.0692(8) 0.7518(4) 0.5820(5) 0.0305(8) Uani 1 1 d D U . . .
H5 H -0.034146 0.775520 0.545895 0.037 Uiso 1 1 calc R U . . .
C6 C 0.1898(8) 0.8114(4) 0.6583(5) 0.0303(8) Uani 1 1 d D U . . .
H6 H 0.167443 0.874272 0.672943 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9730(9) 3_666 ?
Rh1 O3 1.997(4) . ?
Rh1 N1 2.073(4) . ?
Rh1 C2 1.878(5) . ?
Rh1 C1 1.817(5) . ?
Br1 C13 1.883(5) . ?
O3 C3 1.297(6) . ?
N1 C9 1.290(7) . ?
N1 C10 1.437(7) . ?
O2 C2 1.092(6) . ?
C8 C3 1.410(7) . ?
C8 C9 1.433(7) . ?
C8 C7 1.403(7) . ?
C3 C4 1.401(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.129(7) . ?
C13 C12 1.354(9) . ?
C13 C14 1.382(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.358(9) . ?
C15 C14 1.388(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(8) . ?
C10 C11 1.395(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.392(7) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.365(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(7) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.30(15) . 3_666 ?
O3 Rh1 N1 90.68(18) . . ?
N1 Rh1 Rh1 83.17(13) . 3_666 ?
C2 Rh1 Rh1 96.03(19) . 3_666 ?
C2 Rh1 O3 87.1(2) . . ?
C2 Rh1 N1 177.7(2) . . ?
C1 Rh1 Rh1 107.4(2) . 3_666 ?
C1 Rh1 O3 168.7(3) . . ?
C1 Rh1 N1 96.1(2) . . ?
C1 Rh1 C2 86.2(3) . . ?
C3 O3 Rh1 129.5(4) . . ?
C9 N1 Rh1 122.5(4) . . ?
C9 N1 C10 115.7(4) . . ?
C10 N1 Rh1 121.7(4) . . ?
C3 C8 C9 124.3(5) . . ?
C7 C8 C3 119.7(5) . . ?
C7 C8 C9 116.0(5) . . ?
O3 C3 C8 123.6(5) . . ?
O3 C3 C4 118.3(5) . . ?
C4 C3 C8 118.2(5) . . ?
N1 C9 C8 128.9(5) . . ?
N1 C9 H9 115.6 . . ?
C8 C9 H9 115.6 . . ?
C12 C13 Br1 119.7(3) . . ?
C12 C13 C14 121.9(5) . . ?
C14 C13 Br1 118.5(5) . . ?
C10 C15 H15 119.4 . . ?
C10 C15 C14 121.3(5) . . ?
C14 C15 H15 119.4 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(5) . . ?
C5 C4 H4 119.6 . . ?
C15 C10 N1 119.9(4) . . ?
C15 C10 C11 119.7(5) . . ?
C11 C10 N1 120.4(5) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.5(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 C15 118.1(6) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(6) . . ?
C12 C11 H11 120.3 . . ?
O2 C2 Rh1 178.4(6) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 C8 121.0(5) . . ?
C6 C7 H7 119.5 . . ?
O1 C1 Rh1 173.6(7) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.3(5) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.1(5) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -6.5(9) . . . . ?
Rh1 O3 C3 C4 175.1(5) . . . . ?
Rh1 N1 C9 C8 -8.7(9) . . . . ?
Rh1 N1 C10 C15 34.4(8) . . . . ?
Rh1 N1 C10 C11 -145.7(4) . . . . ?
Br1 C13 C12 C11 -179.7(4) . . . . ?
Br1 C13 C14 C15 179.3(4) . . . . ?
O3 C3 C4 C5 177.9(6) . . . . ?
N1 C10 C11 C12 178.9(5) . . . . ?
C8 C3 C4 C5 -0.5(10) . . . . ?
C8 C7 C6 C5 1.0(9) . . . . ?
C3 C8 C9 N1 5.0(11) . . . . ?
C3 C8 C7 C6 -1.6(9) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C9 N1 C10 C15 -147.1(6) . . . . ?
C9 N1 C10 C11 32.8(7) . . . . ?
C9 C8 C3 O3 3.4(10) . . . . ?
C9 C8 C3 C4 -178.2(6) . . . . ?
C9 C8 C7 C6 178.0(6) . . . . ?
C13 C12 C11 C10 0.4(8) . . . . ?
C15 C10 C11 C12 -1.2(8) . . . . ?
C4 C5 C6 C7 -0.2(9) . . . . ?
C10 N1 C9 C8 172.8(6) . . . . ?
C10 C15 C14 C13 0.4(9) . . . . ?
C12 C13 C14 C15 -1.3(9) . . . . ?
C14 C13 C12 C11 0.9(9) . . . . ?
C14 C15 C10 N1 -179.3(5) . . . . ?
C14 C15 C10 C11 0.9(9) . . . . ?
C7 C8 C3 O3 -177.0(6) . . . . ?
C7 C8 C3 C4 1.3(9) . . . . ?
C7 C8 C9 N1 -174.5(6) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.01557000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.720
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-3p92GPa
_database_code_depnum_ccdc_archive 'CCDC 2427957'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-3p92GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.364 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.623(6)
_cell_length_b                   14.461(2)
_cell_length_c                   9.818(11)
_cell_angle_alpha                90
_cell_angle_beta                 105.12(10)
_cell_angle_gamma                90
_cell_volume                     1181.9(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1977
_cell_measurement_theta_min      2.8190
_cell_measurement_theta_max      28.3850

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.835
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.794
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_T_max  0.343
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5491
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.823
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.362
_diffrn_measured_fraction_theta_full 0.364
_diffrn_reflns_Laue_measured_fraction_max 0.362
_diffrn_reflns_Laue_measured_fraction_full 0.364
_diffrn_reflns_point_group_measured_fraction_max 0.362
_diffrn_reflns_point_group_measured_fraction_full 0.364
_reflns_number_total             784
_reflns_number_gt                597
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0811P)²+5.9022P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         784
_refine_ls_number_parameters     190
_refine_ls_number_restraints     278
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1473
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.4787(3) 0.45965(7) 0.6402(3) 0.028(2) Uani 1 1 d D U . . .
Br1 Br 1.3327(3) 0.55451(9) 0.9607(3) 0.0308(18) Uani 1 1 d D U . . .
O3 O 0.2779(18) 0.5355(5) 0.5895(19) 0.0193(13) Uani 1 1 d D U . . .
N1 N 0.607(2) 0.5742(6) 0.735(2) 0.017(4) Uani 1 1 d D U . . .
O2 O 0.288(2) 0.2997(6) 0.504(2) 0.031(6) Uani 1 1 d D U . . .
C8 C 0.381(2) 0.6813(8) 0.682(3) 0.0201(11) Uani 1 1 d D U . . .
O1 O 0.726(2) 0.3176(6) 0.737(2) 0.034(6) Uani 1 1 d D U . . .
C9 C 0.545(2) 0.6536(8) 0.737(3) 0.0191(13) Uani 1 1 d D U . . .
H9 H 0.615158 0.700122 0.779726 0.023 Uiso 1 1 calc R U . . .
C3 C 0.259(2) 0.6228(7) 0.606(3) 0.0202(11) Uani 1 1 d D U . . .
C10 C 0.7787(19) 0.5716(8) 0.784(2) 0.0172(11) Uani 1 1 d D U . . .
C15 C 0.869(2) 0.5183(9) 0.718(2) 0.0171(11) Uani 1 1 d D U . . .
H15 H 0.818670 0.485319 0.637810 0.020 Uiso 1 1 calc R U . . .
C13 C 1.1083(18) 0.5630(8) 0.888(2) 0.0168(11) Uani 1 1 d D U . . .
C11 C 0.856(2) 0.6226(8) 0.9040(19) 0.0173(11) Uani 1 1 d D U . . .
H11 H 0.796062 0.659877 0.948608 0.021 Uiso 1 1 calc R U . . .
C14 C 1.036(2) 0.5124(8) 0.770(2) 0.0169(11) Uani 1 1 d D U . . .
H14 H 1.096003 0.475344 0.725614 0.020 Uiso 1 1 calc R U . . .
C12 C 1.020(2) 0.6175(8) 0.956(2) 0.0173(11) Uani 1 1 d D U . . .
H12 H 1.071857 0.650581 1.036152 0.021 Uiso 1 1 calc R U . . .
C7 C 0.344(2) 0.7737(8) 0.710(3) 0.0202(12) Uani 1 1 d D U . . .
H7 H 0.423656 0.812089 0.762240 0.024 Uiso 1 1 calc R U . . .
C4 C 0.105(2) 0.6600(8) 0.556(3) 0.0203(12) Uani 1 1 d D U . . .
H4 H 0.023312 0.622751 0.503828 0.024 Uiso 1 1 calc R U . . .
C2 C 0.360(3) 0.3592(8) 0.549(3) 0.021(6) Uani 1 1 d D U . . .
C1 C 0.641(3) 0.3767(8) 0.698(3) 0.022(6) Uani 1 1 d D U . . .
C5 C 0.071(3) 0.7498(8) 0.582(3) 0.0204(12) Uani 1 1 d D U . . .
H5 H -0.032502 0.772559 0.547990 0.024 Uiso 1 1 calc R U . . .
C6 C 0.192(2) 0.8069(8) 0.660(2) 0.0204(12) Uani 1 1 d D U . . .
H6 H 0.168256 0.867710 0.678428 0.024 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.818(13) . ?
Rh1 C2 1.864(11) . ?
Rh1 O3 2.000(13) . ?
Rh1 N1 2.072(9) . ?
Rh1 Rh1 3.099(7) 3_666 ?
Br1 C13 1.883(14) . ?
O3 C3 1.289(13) . ?
N1 C9 1.271(15) . ?
N1 C10 1.433(17) . ?
O2 C2 1.086(12) . ?
C8 C3 1.403(14) . ?
C8 C7 1.419(16) . ?
C8 C9 1.430(17) . ?
O1 C1 1.127(13) . ?
C9 H9 0.9300 . ?
C3 C4 1.396(17) . ?
C10 C15 1.372(19) . ?
C10 C11 1.402(15) . ?
C15 C14 1.393(17) . ?
C15 H15 0.9300 . ?
C13 C14 1.377(16) . ?
C13 C12 1.378(18) . ?
C11 C12 1.379(16) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.361(16) . ?
C7 H7 0.9300 . ?
C4 C5 1.369(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(14) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 85.2(7) . . ?
C1 Rh1 O3 170.2(12) . . ?
C2 Rh1 O3 88.7(8) . . ?
C1 Rh1 N1 96.3(5) . . ?
C2 Rh1 N1 177.9(8) . . ?
O3 Rh1 N1 90.0(5) . . ?
C1 Rh1 Rh1 105.5(12) . 3_666 ?
C2 Rh1 Rh1 92.5(11) . 3_666 ?
O3 Rh1 Rh1 82.4(7) . 3_666 ?
N1 Rh1 Rh1 85.6(7) . 3_666 ?
C3 O3 Rh1 129.4(10) . . ?
C9 N1 C10 115.0(12) . . ?
C9 N1 Rh1 123.5(10) . . ?
C10 N1 Rh1 121.0(10) . . ?
C3 C8 C7 119.5(13) . . ?
C3 C8 C9 124.2(12) . . ?
C7 C8 C9 116.3(11) . . ?
N1 C9 C8 128.8(12) . . ?
N1 C9 H9 115.6 . . ?
C8 C9 H9 115.6 . . ?
O3 C3 C4 118.2(12) . . ?
O3 C3 C8 123.7(13) . . ?
C4 C3 C8 117.8(11) . . ?
C15 C10 C11 119.1(13) . . ?
C15 C10 N1 121.4(14) . . ?
C11 C10 N1 119.5(16) . . ?
C10 C15 C14 121.5(14) . . ?
C10 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C14 C13 C12 121.6(14) . . ?
C14 C13 Br1 118.7(13) . . ?
C12 C13 Br1 119.7(10) . . ?
C12 C11 C10 119.9(15) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C14 C15 118.2(16) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C13 C12 C11 119.7(13) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C6 C7 C8 120.7(12) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C5 C4 C3 122.0(12) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
O2 C2 Rh1 175(3) . . ?
O1 C1 Rh1 171(2) . . ?
C4 C5 C6 120.1(14) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 119.9(12) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 173(3) . . . . ?
Rh1 N1 C9 C8 2(4) . . . . ?
C3 C8 C9 N1 -4(5) . . . . ?
C7 C8 C9 N1 175(3) . . . . ?
Rh1 O3 C3 C4 178(2) . . . . ?
Rh1 O3 C3 C8 -8(4) . . . . ?
C7 C8 C3 O3 -172(3) . . . . ?
C9 C8 C3 O3 7(5) . . . . ?
C7 C8 C3 C4 3(4) . . . . ?
C9 C8 C3 C4 -179(3) . . . . ?
C9 N1 C10 C15 -140(2) . . . . ?
Rh1 N1 C10 C15 32(2) . . . . ?
C9 N1 C10 C11 42(3) . . . . ?
Rh1 N1 C10 C11 -146.8(14) . . . . ?
C11 C10 C15 C14 1(2) . . . . ?
N1 C10 C15 C14 -177.2(16) . . . . ?
C15 C10 C11 C12 -1.1(15) . . . . ?
N1 C10 C11 C12 177.3(15) . . . . ?
C12 C13 C14 C15 1(2) . . . . ?
Br1 C13 C14 C15 179.1(13) . . . . ?
C10 C15 C14 C13 -1(2) . . . . ?
C14 C13 C12 C11 -1(2) . . . . ?
Br1 C13 C12 C11 -179.0(10) . . . . ?
C10 C11 C12 C13 0.8(14) . . . . ?
C3 C8 C7 C6 -2(3) . . . . ?
C9 C8 C7 C6 179(2) . . . . ?
O3 C3 C4 C5 173(3) . . . . ?
C8 C3 C4 C5 -2(4) . . . . ?
C3 C4 C5 C6 0(4) . . . . ?
C8 C7 C6 C5 0(2) . . . . ?
C4 C5 C6 C7 0(2) . . . . ?

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.170



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-0p28GPa
_database_code_depnum_ccdc_archive 'CCDC 2427950'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-0p28GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.466 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8641(6)
_cell_length_b                   15.149(8)
_cell_length_c                   10.9081(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.939(8)
_cell_angle_gamma                90
_cell_volume                     1408.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1721
_cell_measurement_theta_min      2.3560
_cell_measurement_theta_max      29.4230

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.057
_shelx_estimated_absorpt_T_min   0.664
_shelx_estimated_absorpt_T_max   0.764
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4087
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.362
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.465
_diffrn_measured_fraction_theta_full 0.466
_diffrn_reflns_Laue_measured_fraction_max 0.465
_diffrn_reflns_Laue_measured_fraction_full 0.466
_diffrn_reflns_point_group_measured_fraction_max 0.465
_diffrn_reflns_point_group_measured_fraction_full 0.466
_reflns_number_total             1199
_reflns_number_gt                976
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+5.9313P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1199
_refine_ls_number_parameters     184
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48127(7) 0.46455(10) 0.64291(6) 0.0311(6) Uani 1 1 d D U . . .
Br1 Br 1.32218(9) 0.55821(14) 0.94726(9) 0.0404(10) Uani 1 1 d D U . . .
O3 O 0.2893(6) 0.5408(8) 0.5799(5) 0.0370(13) Uani 1 1 d D U . . .
N1 N 0.6122(7) 0.5756(9) 0.7205(6) 0.0306(13) Uani 1 1 d D U . . .
O2 O 0.2950(8) 0.3068(10) 0.5249(7) 0.056(3) Uani 1 1 d D U . . .
C8 C 0.3892(9) 0.6801(10) 0.6734(7) 0.0335(9) Uani 1 1 d D U . . .
O1 O 0.7295(9) 0.3335(11) 0.7486(8) 0.078(5) Uani 1 1 d D U . . .
C9 C 0.5527(9) 0.6523(10) 0.7262(7) 0.0315(17) Uani 1 1 d D U . . .
H9 H 0.621817 0.695469 0.769121 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2709(9) 0.6229(9) 0.6015(8) 0.0335(9) Uani 1 1 d D U . . .
C10 C 0.7802(8) 0.5726(10) 0.7759(6) 0.0288(7) Uani 1 1 d D U . . .
C15 C 0.8722(8) 0.5291(10) 0.7111(7) 0.0288(7) Uani 1 1 d D U . . .
H15 H 0.825347 0.502876 0.632818 0.035 Uiso 1 1 calc R U . . .
C13 C 1.1002(8) 0.5644(10) 0.8765(6) 0.0286(7) Uani 1 1 d D U . . .
C11 C 0.8501(8) 0.6109(9) 0.8929(6) 0.0290(7) Uani 1 1 d D U . . .
H11 H 0.788563 0.639562 0.937190 0.035 Uiso 1 1 calc R U . . .
C14 C 1.0333(8) 0.5245(10) 0.7616(6) 0.0288(7) Uani 1 1 d D U . . .
H14 H 1.095069 0.494769 0.718487 0.035 Uiso 1 1 calc R U . . .
C12 C 1.0117(8) 0.6067(9) 0.9445(7) 0.0293(7) Uani 1 1 d D U . . .
H12 H 1.059124 0.631929 1.023412 0.035 Uiso 1 1 calc R U . . .
C7 C 0.3539(9) 0.7670(10) 0.6943(7) 0.0344(9) Uani 1 1 d D U . . .
H7 H 0.433256 0.802735 0.742899 0.041 Uiso 1 1 calc R U . . .
C4 C 0.1203(9) 0.6618(10) 0.5507(7) 0.0343(9) Uani 1 1 d D U . . .
H4 H 0.039728 0.627583 0.500236 0.041 Uiso 1 1 calc R U . . .
C2 C 0.3619(10) 0.3662(10) 0.5702(9) 0.0385(14) Uani 1 1 d D U . . .
C1 C 0.6383(10) 0.3846(11) 0.7094(8) 0.0385(14) Uani 1 1 d D U . . .
C5 C 0.0911(10) 0.7464(10) 0.5735(7) 0.0349(9) Uani 1 1 d D U . . .
H5 H -0.009681 0.768495 0.539459 0.042 Uiso 1 1 calc R U . . .
C6 C 0.2069(9) 0.8026(10) 0.6466(7) 0.0350(9) Uani 1 1 d D U . . .
H6 H 0.185377 0.861028 0.661957 0.042 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.838(12) . ?
Rh1 C2 1.873(13) . ?
Rh1 O3 2.015(8) . ?
Rh1 N1 2.087(11) . ?
Br1 C13 1.908(7) . ?
O3 C3 1.284(14) . ?
N1 C9 1.284(15) . ?
N1 C10 1.446(9) . ?
O2 C2 1.115(14) . ?
C8 C7 1.386(15) . ?
C8 C3 1.420(13) . ?
C8 C9 1.467(11) . ?
O1 C1 1.116(14) . ?
C9 H9 0.9300 . ?
C3 C4 1.425(12) . ?
C10 C11 1.383(10) . ?
C10 C15 1.384(12) . ?
C15 C14 1.385(9) . ?
C15 H15 0.9300 . ?
C13 C14 1.371(11) . ?
C13 C12 1.377(11) . ?
C11 C12 1.389(9) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.374(11) . ?
C7 H7 0.9300 . ?
C4 C5 1.345(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(13) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 85.5(6) . . ?
C1 Rh1 O3 171.8(5) . . ?
C2 Rh1 O3 89.2(4) . . ?
C1 Rh1 N1 95.4(5) . . ?
C2 Rh1 N1 178.8(5) . . ?
O3 Rh1 N1 90.0(4) . . ?
C3 O3 Rh1 129.1(6) . . ?
C9 N1 C10 113.5(10) . . ?
C9 N1 Rh1 124.0(6) . . ?
C10 N1 Rh1 122.6(9) . . ?
C7 C8 C3 120.3(9) . . ?
C7 C8 C9 116.8(10) . . ?
C3 C8 C9 122.8(12) . . ?
N1 C9 C8 128.0(11) . . ?
N1 C9 H9 116.0 . . ?
C8 C9 H9 116.0 . . ?
O3 C3 C8 125.5(9) . . ?
O3 C3 C4 118.8(10) . . ?
C8 C3 C4 115.7(11) . . ?
C11 C10 C15 119.6(7) . . ?
C11 C10 N1 121.4(7) . . ?
C15 C10 N1 119.0(7) . . ?
C10 C15 C14 120.6(8) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C14 C13 C12 122.0(7) . . ?
C14 C13 Br1 119.2(6) . . ?
C12 C13 Br1 118.8(6) . . ?
C10 C11 C12 120.4(8) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C14 C15 118.8(9) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C13 C12 C11 118.6(7) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C6 C7 C8 123.0(10) . . ?
C6 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
C5 C4 C3 122.0(11) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
O2 C2 Rh1 177.5(9) . . ?
O1 C1 Rh1 177.3(13) . . ?
C4 C5 C6 122.4(10) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 116.5(12) . . ?
C7 C6 H6 121.7 . . ?
C5 C6 H6 121.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 176.2(7) . . . . ?
Rh1 N1 C9 C8 -5.0(13) . . . . ?
C7 C8 C9 N1 179.0(9) . . . . ?
C3 C8 C9 N1 -2.3(14) . . . . ?
Rh1 O3 C3 C8 2.8(14) . . . . ?
Rh1 O3 C3 C4 -177.1(5) . . . . ?
C7 C8 C3 O3 -177.6(9) . . . . ?
C9 C8 C3 O3 3.7(15) . . . . ?
C7 C8 C3 C4 2.3(13) . . . . ?
C9 C8 C3 C4 -176.4(8) . . . . ?
C9 N1 C10 C11 45.8(13) . . . . ?
Rh1 N1 C10 C11 -132.9(9) . . . . ?
C9 N1 C10 C15 -135.2(11) . . . . ?
Rh1 N1 C10 C15 46.1(13) . . . . ?
C11 C10 C15 C14 -0.6(18) . . . . ?
N1 C10 C15 C14 -179.6(13) . . . . ?
C15 C10 C11 C12 0.7(13) . . . . ?
N1 C10 C11 C12 179.7(12) . . . . ?
C12 C13 C14 C15 2(2) . . . . ?
Br1 C13 C14 C15 179.9(11) . . . . ?
C10 C15 C14 C13 -1(2) . . . . ?
C14 C13 C12 C11 -1.8(17) . . . . ?
Br1 C13 C12 C11 -179.8(8) . . . . ?
C10 C11 C12 C13 0.5(12) . . . . ?
C3 C8 C7 C6 -1.0(13) . . . . ?
C9 C8 C7 C6 177.7(7) . . . . ?
O3 C3 C4 C5 177.5(9) . . . . ?
C8 C3 C4 C5 -2.4(13) . . . . ?
C3 C4 C5 C6 1.2(14) . . . . ?
C8 C7 C6 C5 -0.3(11) . . . . ?
C4 C5 C6 C7 0.2(11) . . . . ?

_refine_diff_density_max         0.506
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.084



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-3p36GPa
_database_code_depnum_ccdc_archive 'CCDC 2427956'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-3p36GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.371 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.623(6)
_cell_length_b                   14.510(3)
_cell_length_c                   9.931(11)
_cell_angle_alpha                90
_cell_angle_beta                 104.91(11)
_cell_angle_gamma                90
_cell_volume                     1200.7(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1280
_cell_measurement_theta_min      2.8120
_cell_measurement_theta_max      26.5410

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.759
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.797
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_T_max  0.255
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3200
_diffrn_reflns_av_unetI/netI     0.1204
_diffrn_reflns_av_R_equivalents  0.1036
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.545
_diffrn_reflns_theta_max         25.329
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.371
_diffrn_measured_fraction_theta_full 0.371
_diffrn_reflns_Laue_measured_fraction_max 0.371
_diffrn_reflns_Laue_measured_fraction_full 0.371
_diffrn_reflns_point_group_measured_fraction_max 0.371
_diffrn_reflns_point_group_measured_fraction_full 0.371
_reflns_number_total             814
_reflns_number_gt                570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0983P)²+16.1671P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         814
_refine_ls_number_parameters     190
_refine_ls_number_restraints     278
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.2014
_refine_ls_wR_factor_gt          0.1619
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.4789(3) 0.45991(10) 0.6395(3) 0.030(3) Uani 1 1 d D U . . .
Br1 Br 1.3317(4) 0.55486(13) 0.9602(5) 0.029(2) Uani 1 1 d D U . . .
O3 O 0.276(2) 0.5352(7) 0.592(2) 0.023(12) Uani 1 1 d D U . . .
N1 N 0.608(2) 0.5734(8) 0.731(3) 0.016(5) Uani 1 1 d D U . . .
O2 O 0.290(3) 0.2988(8) 0.504(3) 0.037(11) Uani 1 1 d D U . . .
C8 C 0.384(3) 0.6810(11) 0.679(3) 0.0191(14) Uani 1 1 d D U . . .
O1 O 0.724(3) 0.3195(8) 0.738(3) 0.032(10) Uani 1 1 d D U . . .
C9 C 0.547(3) 0.6540(11) 0.736(4) 0.0185(15) Uani 1 1 d D U . . .
H9 H 0.616119 0.699553 0.781941 0.022 Uiso 1 1 calc R U . . .
C3 C 0.261(3) 0.6232(9) 0.608(3) 0.0192(14) Uani 1 1 d D U . . .
C10 C 0.779(2) 0.5705(11) 0.787(2) 0.0156(13) Uani 1 1 d D U . . .
C15 C 0.871(2) 0.5189(12) 0.719(2) 0.0155(13) Uani 1 1 d D U . . .
H15 H 0.821485 0.487624 0.637845 0.019 Uiso 1 1 calc R U . . .
C13 C 1.106(2) 0.5617(11) 0.890(2) 0.0152(13) Uani 1 1 d D U . . .
C11 C 0.853(2) 0.6198(10) 0.906(2) 0.0156(13) Uani 1 1 d D U . . .
H11 H 0.791700 0.655456 0.951012 0.019 Uiso 1 1 calc R U . . .
C14 C 1.036(2) 0.5133(11) 0.772(2) 0.0155(13) Uani 1 1 d D U . . .
H14 H 1.097583 0.477376 0.727676 0.019 Uiso 1 1 calc R U . . .
C12 C 1.019(2) 0.6152(10) 0.957(2) 0.0156(13) Uani 1 1 d D U . . .
H12 H 1.069582 0.648014 1.036893 0.019 Uiso 1 1 calc R U . . .
C7 C 0.350(3) 0.7741(10) 0.704(3) 0.0193(14) Uani 1 1 d D U . . .
H7 H 0.431319 0.812085 0.754398 0.023 Uiso 1 1 calc R U . . .
C4 C 0.107(3) 0.6607(10) 0.555(3) 0.0193(14) Uani 1 1 d D U . . .
H4 H 0.025090 0.624102 0.502662 0.023 Uiso 1 1 calc R U . . .
C2 C 0.360(4) 0.3597(10) 0.552(4) 0.020(6) Uani 1 1 d D U . . .
C1 C 0.641(3) 0.3775(11) 0.691(4) 0.015(6) Uani 1 1 d D U . . .
C5 C 0.077(3) 0.7506(10) 0.581(3) 0.0194(14) Uani 1 1 d D U . . .
H5 H -0.026650 0.773836 0.548763 0.023 Uiso 1 1 calc R U . . .
C6 C 0.199(3) 0.8082(11) 0.655(3) 0.0194(14) Uani 1 1 d D U . . .
H6 H 0.177694 0.869519 0.671167 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.811(16) . ?
Rh1 C2 1.862(13) . ?
Rh1 O3 2.010(15) . ?
Rh1 N1 2.063(12) . ?
Rh1 Rh1 3.111(8) 3_666 ?
Br1 C13 1.892(16) . ?
O3 C3 1.298(15) . ?
N1 C9 1.290(18) . ?
N1 C10 1.432(18) . ?
O2 C2 1.107(14) . ?
C8 C3 1.399(16) . ?
C8 C7 1.419(17) . ?
C8 C9 1.422(19) . ?
O1 C1 1.126(14) . ?
C9 H9 0.9300 . ?
C3 C4 1.401(18) . ?
C10 C15 1.382(19) . ?
C10 C11 1.391(17) . ?
C15 C14 1.388(18) . ?
C15 H15 0.9300 . ?
C13 C14 1.365(18) . ?
C13 C12 1.376(19) . ?
C11 C12 1.391(17) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.358(17) . ?
C7 H7 0.9300 . ?
C4 C5 1.368(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(17) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 84.8(10) . . ?
C1 Rh1 O3 170.4(13) . . ?
C2 Rh1 O3 88.6(10) . . ?
C1 Rh1 N1 96.4(7) . . ?
C2 Rh1 N1 178.1(12) . . ?
O3 Rh1 N1 90.4(6) . . ?
C1 Rh1 Rh1 103.9(15) . 3_666 ?
C2 Rh1 Rh1 92.9(15) . 3_666 ?
O3 Rh1 Rh1 83.3(8) . 3_666 ?
N1 Rh1 Rh1 85.4(9) . 3_666 ?
C3 O3 Rh1 128.3(13) . . ?
C9 N1 C10 113.8(14) . . ?
C9 N1 Rh1 124.0(13) . . ?
C10 N1 Rh1 122.0(11) . . ?
C3 C8 C7 119.5(15) . . ?
C3 C8 C9 125.5(15) . . ?
C7 C8 C9 114.9(14) . . ?
N1 C9 C8 127.3(16) . . ?
N1 C9 H9 116.3 . . ?
C8 C9 H9 116.3 . . ?
O3 C3 C8 124.0(15) . . ?
O3 C3 C4 117.2(14) . . ?
C8 C3 C4 118.7(13) . . ?
C15 C10 C11 119.7(16) . . ?
C15 C10 N1 119.4(18) . . ?
C11 C10 N1 120.9(19) . . ?
C10 C15 C14 120.9(17) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C14 C13 C12 122.1(16) . . ?
C14 C13 Br1 118.6(15) . . ?
C12 C13 Br1 119.4(12) . . ?
C10 C11 C12 119.4(17) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C14 C15 118.5(18) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C13 C12 C11 119.4(16) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C6 C7 C8 120.6(15) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C5 C4 C3 120.6(14) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
O2 C2 Rh1 178(3) . . ?
O1 C1 Rh1 167(4) . . ?
C4 C5 C6 120.9(16) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 119.6(16) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 174(3) . . . . ?
Rh1 N1 C9 C8 -2(6) . . . . ?
C3 C8 C9 N1 1(6) . . . . ?
C7 C8 C9 N1 178(4) . . . . ?
Rh1 O3 C3 C8 -9(5) . . . . ?
Rh1 O3 C3 C4 175(2) . . . . ?
C7 C8 C3 O3 -172(4) . . . . ?
C9 C8 C3 O3 5(6) . . . . ?
C7 C8 C3 C4 4(5) . . . . ?
C9 C8 C3 C4 -179(4) . . . . ?
C9 N1 C10 C15 -139(3) . . . . ?
Rh1 N1 C10 C15 37(3) . . . . ?
C9 N1 C10 C11 40(4) . . . . ?
Rh1 N1 C10 C11 -144.2(18) . . . . ?
C11 C10 C15 C14 2(3) . . . . ?
N1 C10 C15 C14 -179(2) . . . . ?
C15 C10 C11 C12 -1.1(17) . . . . ?
N1 C10 C11 C12 179.9(19) . . . . ?
C12 C13 C14 C15 0(3) . . . . ?
Br1 C13 C14 C15 -179.5(17) . . . . ?
C10 C15 C14 C13 -2(3) . . . . ?
C14 C13 C12 C11 1(3) . . . . ?
Br1 C13 C12 C11 -179.6(12) . . . . ?
C10 C11 C12 C13 -0.3(15) . . . . ?
C3 C8 C7 C6 -2(4) . . . . ?
C9 C8 C7 C6 -180(3) . . . . ?
O3 C3 C4 C5 173(3) . . . . ?
C8 C3 C4 C5 -4(5) . . . . ?
C2 Rh1 C1 O1 -68(9) . . . . ?
N1 Rh1 C1 O1 113(9) . . . . ?
Rh1 Rh1 C1 O1 -160(8) 3_666 . . . ?
C3 C4 C5 C6 2(4) . . . . ?
C8 C7 C6 C5 1(2) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?

_refine_diff_density_max         1.009
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.193



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-19-HP-ESRF-9p87GPa
_database_code_depnum_ccdc_archive 'CCDC 2427945'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-19-HP-ESRF-9p87GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.437 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4031(7)
_cell_length_b                   14.0258(13)
_cell_length_c                   9.0664(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.615(9)
_cell_angle_gamma                90
_cell_volume                     1042.78(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    588
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.9520
_cell_measurement_theta_min      2.3060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.437
_diffrn_reflns_Laue_measured_fraction_max 0.375
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2260
_diffrn_reflns_point_group_measured_fraction_full 0.437
_diffrn_reflns_point_group_measured_fraction_max 0.375
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.798
_diffrn_reflns_theta_min         2.136
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.437
_diffrn_measured_fraction_theta_max 0.375
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0292410000
_diffrn_orient_matrix_UB_12      0.0165947000
_diffrn_orient_matrix_UB_13      0.0202901000
_diffrn_orient_matrix_UB_21      0.0285267000
_diffrn_orient_matrix_UB_22      -0.0063327000
_diffrn_orient_matrix_UB_23      0.0414852000
_diffrn_orient_matrix_UB_31      0.0286514000
_diffrn_orient_matrix_UB_32      0.0231877000
_diffrn_orient_matrix_UB_33      -0.0030614000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1200
_reflns_number_total             1363
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1363
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0732P)²+5.3682P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1331
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47908(9) 0.45623(5) 0.63819(7) 0.0344(3) Uani 1 1 d D U . . .
Br1 Br 1.33762(11) 0.55353(6) 0.97000(9) 0.0351(3) Uani 1 1 d D U . . .
O3 O 0.2726(9) 0.5307(5) 0.5930(7) 0.0391(17) Uani 1 1 d D U . . .
N1 N 0.6090(9) 0.5748(5) 0.7302(7) 0.0323(14) Uani 1 1 d D U . . .
O2 O 0.2756(11) 0.2951(5) 0.4936(9) 0.051(3) Uani 1 1 d D U . . .
C8 C 0.3736(11) 0.6814(6) 0.6877(9) 0.0347(11) Uani 1 1 d D U . . .
C3 C 0.2503(11) 0.6195(6) 0.6123(9) 0.0347(11) Uani 1 1 d D U . . .
C9 C 0.5392(11) 0.6545(6) 0.7461(9) 0.0333(19) Uani 1 1 d D U . . .
H9 H 0.605050 0.700606 0.802973 0.040 Uiso 1 1 calc R U . . .
O1 O 0.7359(11) 0.3134(5) 0.7354(8) 0.051(3) Uani 1 1 d D U . . .
C13 C 1.1105(10) 0.5621(6) 0.8965(9) 0.0355(9) Uani 1 1 d D U . . .
C15 C 0.8755(10) 0.5116(6) 0.7214(9) 0.0354(9) Uani 1 1 d D U . . .
H15 H 0.825286 0.473846 0.640151 0.042 Uiso 1 1 calc R U . . .
C4 C 0.0935(11) 0.6581(6) 0.5579(9) 0.0352(11) Uani 1 1 d D U . . .
H4 H 0.009831 0.619136 0.506966 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7835(10) 0.5716(6) 0.7848(9) 0.0355(9) Uani 1 1 d D U . . .
C12 C 1.0232(10) 0.6239(6) 0.9611(9) 0.0359(9) Uani 1 1 d D U . . .
H12 H 1.073863 0.661755 1.041976 0.043 Uiso 1 1 calc R U . . .
C14 C 1.0430(10) 0.5050(6) 0.7747(9) 0.0354(9) Uani 1 1 d D U . . .
H14 H 1.106534 0.464239 0.730695 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8564(10) 0.6297(6) 0.9042(8) 0.0360(9) Uani 1 1 d D U . . .
H11 H 0.793772 0.672376 0.945841 0.043 Uiso 1 1 calc R U . . .
C2 C 0.3542(13) 0.3526(6) 0.5489(10) 0.039(3) Uani 1 1 d D U . . .
C7 C 0.3372(11) 0.7754(6) 0.7104(9) 0.0352(11) Uani 1 1 d D U . . .
H7 H 0.417916 0.815025 0.764753 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6442(11) 0.3711(6) 0.6957(9) 0.035(2) Uani 1 1 d D U . . .
C5 C 0.0637(11) 0.7514(6) 0.5791(9) 0.0357(11) Uani 1 1 d D U . . .
H5 H -0.040543 0.775337 0.542005 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1841(11) 0.8118(6) 0.6543(9) 0.0357(11) Uani 1 1 d D U . . .
H6 H 0.161956 0.875891 0.666822 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.8801(16) 3_666 ?
Rh1 O3 1.990(7) . ?
Rh1 N1 2.063(6) . ?
Rh1 C2 1.871(7) . ?
Rh1 C1 1.818(8) . ?
Br1 C13 1.883(8) . ?
O3 C3 1.277(10) . ?
N1 C9 1.285(11) . ?
N1 C10 1.442(10) . ?
O2 C2 1.092(9) . ?
C8 C3 1.410(10) . ?
C8 C9 1.427(10) . ?
C8 C7 1.380(11) . ?
C3 C4 1.410(11) . ?
C9 H9 0.9300 . ?
O1 C1 1.121(9) . ?
C13 C12 1.349(12) . ?
C13 C14 1.381(10) . ?
C15 H15 0.9300 . ?
C15 C10 1.353(12) . ?
C15 C14 1.388(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.353(11) . ?
C10 C11 1.387(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.386(10) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.374(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.380(10) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.2(2) . 3_666 ?
O3 Rh1 N1 91.2(3) . . ?
N1 Rh1 Rh1 81.6(2) . 3_666 ?
C2 Rh1 Rh1 96.8(3) . 3_666 ?
C2 Rh1 O3 86.4(4) . . ?
C2 Rh1 N1 177.3(3) . . ?
C1 Rh1 Rh1 107.4(4) . 3_666 ?
C1 Rh1 O3 168.6(4) . . ?
C1 Rh1 N1 96.3(3) . . ?
C1 Rh1 C2 86.2(4) . . ?
C3 O3 Rh1 129.1(5) . . ?
C9 N1 Rh1 122.2(6) . . ?
C9 N1 C10 116.3(7) . . ?
C10 N1 Rh1 121.4(6) . . ?
C3 C8 C9 124.8(8) . . ?
C7 C8 C3 119.9(7) . . ?
C7 C8 C9 115.3(7) . . ?
O3 C3 C8 123.6(7) . . ?
O3 C3 C4 118.8(7) . . ?
C8 C3 C4 117.7(7) . . ?
N1 C9 C8 128.3(7) . . ?
N1 C9 H9 115.8 . . ?
C8 C9 H9 115.8 . . ?
C12 C13 Br1 119.5(5) . . ?
C12 C13 C14 123.5(7) . . ?
C14 C13 Br1 117.0(7) . . ?
C10 C15 H15 119.2 . . ?
C10 C15 C14 121.6(7) . . ?
C14 C15 H15 119.2 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.7 . . ?
C15 C10 N1 120.5(7) . . ?
C15 C10 C11 120.1(8) . . ?
C11 C10 N1 119.5(8) . . ?
C13 C12 H12 120.7 . . ?
C13 C12 C11 118.5(7) . . ?
C11 C12 H12 120.7 . . ?
C13 C14 C15 116.6(9) . . ?
C13 C14 H14 121.7 . . ?
C15 C14 H14 121.7 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(9) . . ?
C12 C11 H11 120.2 . . ?
O2 C2 Rh1 176.5(9) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.3(7) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 173.6(10) . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.7(7) . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 118.7(8) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -7.2(15) . . . . ?
Rh1 O3 C3 C4 174.0(7) . . . . ?
Rh1 N1 C9 C8 -9.9(14) . . . . ?
Rh1 N1 C10 C15 30.1(12) . . . . ?
Rh1 N1 C10 C11 -149.2(6) . . . . ?
Br1 C13 C12 C11 179.4(6) . . . . ?
Br1 C13 C14 C15 179.9(7) . . . . ?
O3 C3 C4 C5 178.4(9) . . . . ?
N1 C10 C11 C12 177.3(8) . . . . ?
C8 C3 C4 C5 -0.5(15) . . . . ?
C8 C7 C6 C5 2.5(12) . . . . ?
C3 C8 C9 N1 6.7(17) . . . . ?
C3 C8 C7 C6 -3.2(14) . . . . ?
C3 C4 C5 C6 -0.2(15) . . . . ?
C9 N1 C10 C15 -151.8(9) . . . . ?
C9 N1 C10 C11 28.9(12) . . . . ?
C9 C8 C3 O3 2.8(16) . . . . ?
C9 C8 C3 C4 -178.3(10) . . . . ?
C9 C8 C7 C6 177.2(9) . . . . ?
C13 C12 C11 C10 0.9(11) . . . . ?
C15 C10 C11 C12 -2.0(11) . . . . ?
C4 C5 C6 C7 -0.8(12) . . . . ?
C10 N1 C9 C8 172.0(10) . . . . ?
C10 C15 C14 C13 0.6(15) . . . . ?
C12 C13 C14 C15 -1.7(16) . . . . ?
C14 C13 C12 C11 1.0(15) . . . . ?
C14 C15 C10 N1 -178.0(8) . . . . ?
C14 C15 C10 C11 1.2(15) . . . . ?
C7 C8 C3 O3 -176.7(9) . . . . ?
C7 C8 C3 C4 2.1(14) . . . . ?
C7 C8 C9 N1 -173.7(10) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00592000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.879
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-0p00GPa
_database_code_depnum_ccdc_archive 'CCDC 2427952'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-0p00GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.467 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.9123(6)
_cell_length_b                   15.285(7)
_cell_length_c                   11.1407(11)
_cell_angle_alpha                90
_cell_angle_beta                 106.234(8)
_cell_angle_gamma                90
_cell_volume                     1457.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1839
_cell_measurement_theta_min      2.9250
_cell_measurement_theta_max      27.4360

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    3.922
_shelx_estimated_absorpt_T_min   0.672
_shelx_estimated_absorpt_T_max   0.771
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_T_max  0.340
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4574
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.324
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.466
_diffrn_measured_fraction_theta_full 0.467
_diffrn_reflns_Laue_measured_fraction_max 0.466
_diffrn_reflns_Laue_measured_fraction_full 0.467
_diffrn_reflns_point_group_measured_fraction_max 0.466
_diffrn_reflns_point_group_measured_fraction_full 0.467
_reflns_number_total             1247
_reflns_number_gt                985
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+4.6521P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1247
_refine_ls_number_parameters     184
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1191
_refine_ls_wR_factor_gt          0.1083
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48184(7) 0.46584(10) 0.64345(6) 0.0349(6) Uani 1 1 d D U . . .
Br1 Br 1.32020(10) 0.55854(15) 0.94441(10) 0.0473(11) Uani 1 1 d D U . . .
O3 O 0.2909(7) 0.5421(8) 0.5796(5) 0.0409(14) Uani 1 1 d D U . . .
N1 N 0.6132(8) 0.5764(9) 0.7184(6) 0.0351(15) Uani 1 1 d D U . . .
O2 O 0.2951(9) 0.3095(10) 0.5303(7) 0.064(4) Uani 1 1 d D U . . .
C8 C 0.3913(9) 0.6792(10) 0.6708(7) 0.0377(9) Uani 1 1 d D U . . .
O1 O 0.7311(9) 0.3365(12) 0.7487(9) 0.091(5) Uani 1 1 d D U . . .
C9 C 0.5533(10) 0.6522(11) 0.7227(8) 0.0347(17) Uani 1 1 d D U . . .
H9 H 0.621887 0.695365 0.764129 0.042 Uiso 1 1 calc R U . . .
C3 C 0.2723(10) 0.6237(10) 0.5989(8) 0.0375(9) Uani 1 1 d D U . . .
C10 C 0.7798(8) 0.5725(10) 0.7738(7) 0.0315(8) Uani 1 1 d D U . . .
C15 C 0.8715(9) 0.5298(10) 0.7103(7) 0.0315(8) Uani 1 1 d D U . . .
H15 H 0.824630 0.503320 0.633857 0.038 Uiso 1 1 calc R U . . .
C13 C 1.0996(8) 0.5648(10) 0.8744(7) 0.0314(7) Uani 1 1 d D U . . .
C11 C 0.8493(9) 0.6098(9) 0.8903(7) 0.0319(8) Uani 1 1 d D U . . .
H11 H 0.788166 0.637553 0.934151 0.038 Uiso 1 1 calc R U . . .
C14 C 1.0331(9) 0.5261(11) 0.7599(7) 0.0315(8) Uani 1 1 d D U . . .
H14 H 1.094890 0.498108 0.716755 0.038 Uiso 1 1 calc R U . . .
C12 C 1.0103(8) 0.6054(9) 0.9404(7) 0.0322(8) Uani 1 1 d D U . . .
H12 H 1.057435 0.629911 1.018266 0.039 Uiso 1 1 calc R U . . .
C7 C 0.3563(10) 0.7660(10) 0.6902(7) 0.0385(9) Uani 1 1 d D U . . .
H7 H 0.435169 0.801968 0.737274 0.046 Uiso 1 1 calc R U . . .
C4 C 0.1224(10) 0.6611(10) 0.5491(8) 0.0383(9) Uani 1 1 d D U . . .
H4 H 0.042029 0.626935 0.500238 0.046 Uiso 1 1 calc R U . . .
C2 C 0.3611(10) 0.3677(10) 0.5741(9) 0.0422(15) Uani 1 1 d D U . . .
C1 C 0.6406(10) 0.3872(11) 0.7085(9) 0.0422(15) Uani 1 1 d D U . . .
C5 C 0.0940(10) 0.7448(10) 0.5711(7) 0.0389(9) Uani 1 1 d D U . . .
H5 H -0.006571 0.766467 0.537673 0.047 Uiso 1 1 calc R U . . .
C6 C 0.2081(9) 0.8005(10) 0.6415(7) 0.0390(9) Uani 1 1 d D U . . .
H6 H 0.185895 0.858499 0.655430 0.047 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.844(12) . ?
Rh1 C2 1.881(13) . ?
Rh1 O3 2.021(8) . ?
Rh1 N1 2.092(11) . ?
Br1 C13 1.904(7) . ?
O3 C3 1.284(15) . ?
N1 C9 1.281(15) . ?
N1 C10 1.441(9) . ?
O2 C2 1.102(14) . ?
C8 C7 1.394(15) . ?
C8 C3 1.418(13) . ?
C8 C9 1.457(11) . ?
O1 C1 1.118(14) . ?
C9 H9 0.9300 . ?
C3 C4 1.416(12) . ?
C10 C15 1.384(12) . ?
C10 C11 1.395(11) . ?
C15 C14 1.392(10) . ?
C15 H15 0.9300 . ?
C13 C12 1.374(12) . ?
C13 C14 1.381(11) . ?
C11 C12 1.388(10) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.384(12) . ?
C7 H7 0.9300 . ?
C4 C5 1.338(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(13) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 86.0(6) . . ?
C1 Rh1 O3 173.1(5) . . ?
C2 Rh1 O3 89.2(5) . . ?
C1 Rh1 N1 95.0(5) . . ?
C2 Rh1 N1 179.0(5) . . ?
O3 Rh1 N1 89.8(4) . . ?
C3 O3 Rh1 129.6(7) . . ?
C9 N1 C10 114.3(11) . . ?
C9 N1 Rh1 123.5(7) . . ?
C10 N1 Rh1 122.1(10) . . ?
C7 C8 C3 119.5(9) . . ?
C7 C8 C9 116.6(11) . . ?
C3 C8 C9 123.8(12) . . ?
N1 C9 C8 128.2(12) . . ?
N1 C9 H9 115.9 . . ?
C8 C9 H9 115.9 . . ?
O3 C3 C4 118.6(10) . . ?
O3 C3 C8 124.3(10) . . ?
C4 C3 C8 117.0(12) . . ?
C15 C10 C11 119.7(7) . . ?
C15 C10 N1 119.1(8) . . ?
C11 C10 N1 121.2(8) . . ?
C10 C15 C14 120.7(9) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C12 C13 C14 121.7(7) . . ?
C12 C13 Br1 119.3(6) . . ?
C14 C13 Br1 119.0(7) . . ?
C12 C11 C10 119.7(8) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C14 C15 118.6(9) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C13 C12 C11 119.6(8) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C6 C7 C8 122.2(11) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C5 C4 C3 121.4(11) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
O2 C2 Rh1 176.7(10) . . ?
O1 C1 Rh1 176.3(13) . . ?
C4 C5 C6 122.9(10) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C7 C6 C5 117.1(12) . . ?
C7 C6 H6 121.5 . . ?
C5 C6 H6 121.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 177.0(8) . . . . ?
Rh1 N1 C9 C8 -5.0(14) . . . . ?
C7 C8 C9 N1 179.2(9) . . . . ?
C3 C8 C9 N1 -3.6(16) . . . . ?
Rh1 O3 C3 C4 -176.1(6) . . . . ?
Rh1 O3 C3 C8 1.6(15) . . . . ?
C7 C8 C3 O3 -177.2(9) . . . . ?
C9 C8 C3 O3 5.7(16) . . . . ?
C7 C8 C3 C4 0.5(14) . . . . ?
C9 C8 C3 C4 -176.5(8) . . . . ?
C9 N1 C10 C15 -134.3(11) . . . . ?
Rh1 N1 C10 C15 47.7(13) . . . . ?
C9 N1 C10 C11 46.5(14) . . . . ?
Rh1 N1 C10 C11 -131.5(9) . . . . ?
C11 C10 C15 C14 -2.0(18) . . . . ?
N1 C10 C15 C14 178.8(14) . . . . ?
C15 C10 C11 C12 1.3(13) . . . . ?
N1 C10 C11 C12 -179.5(12) . . . . ?
C12 C13 C14 C15 1(2) . . . . ?
Br1 C13 C14 C15 179.0(12) . . . . ?
C10 C15 C14 C13 1(2) . . . . ?
C14 C13 C12 C11 -1.5(17) . . . . ?
Br1 C13 C12 C11 -179.7(9) . . . . ?
C10 C11 C12 C13 0.4(12) . . . . ?
C3 C8 C7 C6 0.2(13) . . . . ?
C9 C8 C7 C6 177.5(7) . . . . ?
O3 C3 C4 C5 176.8(9) . . . . ?
C8 C3 C4 C5 -1.1(14) . . . . ?
C3 C4 C5 C6 1.0(15) . . . . ?
C8 C7 C6 C5 -0.4(11) . . . . ?
C4 C5 C6 C7 -0.2(12) . . . . ?

_refine_diff_density_max         0.448
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.091



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-11-HP-ESRF-5p01GPa
_database_code_depnum_ccdc_archive 'CCDC 2427947'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-11-HP-ESRF-5p01GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.455 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5932(5)
_cell_length_b                   14.2844(7)
_cell_length_c                   9.6466(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.168(5)
_cell_angle_gamma                90
_cell_volume                     1148.08(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1079
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.5590
_cell_measurement_theta_min      2.1010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.455
_diffrn_reflns_Laue_measured_fraction_max 0.389
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2582
_diffrn_reflns_point_group_measured_fraction_full 0.455
_diffrn_reflns_point_group_measured_fraction_max 0.389
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.794
_diffrn_reflns_theta_min         2.068
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.455
_diffrn_measured_fraction_theta_max 0.389
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0285721000
_diffrn_orient_matrix_UB_12      0.0160585000
_diffrn_orient_matrix_UB_13      0.0187401000
_diffrn_orient_matrix_UB_21      0.0269220000
_diffrn_orient_matrix_UB_22      -0.0076047000
_diffrn_orient_matrix_UB_23      0.0395740000
_diffrn_orient_matrix_UB_31      0.0296003000
_diffrn_orient_matrix_UB_32      0.0224773000
_diffrn_orient_matrix_UB_33      -0.0000646000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1435
_reflns_number_total             1553
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1553
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+2.5297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0892
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47953(6) 0.45778(3) 0.63783(4) 0.02492(15) Uani 1 1 d D U . . .
Br1 Br 1.33303(7) 0.55488(4) 0.96404(5) 0.02833(18) Uani 1 1 d D U . . .
O3 O 0.2770(5) 0.5334(3) 0.5897(4) 0.0305(10) Uani 1 1 d D U . . .
N1 N 0.6104(6) 0.5739(3) 0.7299(4) 0.0237(8) Uani 1 1 d D U . . .
O2 O 0.2837(7) 0.2958(3) 0.4987(5) 0.0423(15) Uani 1 1 d D U . . .
C8 C 0.3798(7) 0.6816(3) 0.6864(5) 0.0262(7) Uani 1 1 d D U . . .
C3 C 0.2564(7) 0.6216(3) 0.6113(5) 0.0265(7) Uani 1 1 d D U . . .
C9 C 0.5425(7) 0.6536(3) 0.7437(5) 0.0254(11) Uani 1 1 d D U . . .
H9 H 0.608812 0.698447 0.798180 0.030 Uiso 1 1 calc R U . . .
O1 O 0.7317(7) 0.3154(3) 0.7362(5) 0.0433(15) Uani 1 1 d D U . . .
C13 C 1.1093(7) 0.5632(4) 0.8915(5) 0.0266(6) Uani 1 1 d D U . . .
C15 C 0.8729(7) 0.5178(4) 0.7180(5) 0.0266(6) Uani 1 1 d D U . . .
H15 H 0.823901 0.484781 0.635753 0.032 Uiso 1 1 calc R U . . .
C4 C 0.1027(7) 0.6601(4) 0.5584(5) 0.0281(7) Uani 1 1 d D U . . .
H4 H 0.020965 0.622358 0.506118 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7807(7) 0.5704(4) 0.7854(5) 0.0266(6) Uani 1 1 d D U . . .
C12 C 1.0206(7) 0.6170(3) 0.9605(5) 0.0270(6) Uani 1 1 d D U . . .
H12 H 1.070544 0.650237 1.042198 0.032 Uiso 1 1 calc R U . . .
C14 C 1.0378(7) 0.5127(4) 0.7697(5) 0.0267(6) Uani 1 1 d D U . . .
H14 H 1.099436 0.476075 0.723718 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8546(6) 0.6219(3) 0.9074(5) 0.0272(6) Uani 1 1 d D U . . .
H11 H 0.793282 0.659062 0.952773 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3554(7) 0.3552(4) 0.5516(5) 0.0307(15) Uani 1 1 d D U . . .
C7 C 0.3418(7) 0.7755(3) 0.7110(5) 0.0273(7) Uani 1 1 d D U . . .
H7 H 0.421393 0.814220 0.764068 0.033 Uiso 1 1 calc R U . . .
C1 C 0.6420(7) 0.3735(4) 0.6972(5) 0.0292(13) Uani 1 1 d D U . . .
C5 C 0.0708(7) 0.7516(4) 0.5822(5) 0.0291(7) Uani 1 1 d D U . . .
H5 H -0.032331 0.775065 0.547104 0.035 Uiso 1 1 calc R U . . .
C6 C 0.1919(7) 0.8103(4) 0.6589(5) 0.0286(7) Uani 1 1 d D U . . .
H6 H 0.169988 0.872719 0.674035 0.034 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 3.0178(9) 3_666 ?
Rh1 O3 2.003(4) . ?
Rh1 N1 2.077(4) . ?
Rh1 C2 1.882(5) . ?
Rh1 C1 1.826(5) . ?
Br1 C13 1.882(5) . ?
O3 C3 1.297(6) . ?
N1 C9 1.302(7) . ?
N1 C10 1.431(7) . ?
O2 C2 1.098(6) . ?
C8 C3 1.416(7) . ?
C8 C9 1.429(7) . ?
C8 C7 1.414(7) . ?
C3 C4 1.405(7) . ?
C9 H9 0.9300 . ?
O1 C1 1.133(6) . ?
C13 C12 1.364(8) . ?
C13 C14 1.388(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.367(8) . ?
C15 C14 1.384(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(7) . ?
C10 C11 1.401(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.394(7) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.357(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.399(7) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.10(14) . 3_666 ?
O3 Rh1 N1 91.00(17) . . ?
N1 Rh1 Rh1 83.69(12) . 3_666 ?
C2 Rh1 Rh1 95.59(18) . 3_666 ?
C2 Rh1 O3 87.2(2) . . ?
C2 Rh1 N1 178.13(19) . . ?
C1 Rh1 Rh1 107.1(2) . 3_666 ?
C1 Rh1 O3 169.1(3) . . ?
C1 Rh1 N1 95.75(19) . . ?
C1 Rh1 C2 86.1(2) . . ?
C3 O3 Rh1 129.2(3) . . ?
C9 N1 Rh1 122.2(4) . . ?
C9 N1 C10 115.8(4) . . ?
C10 N1 Rh1 122.0(3) . . ?
C3 C8 C9 124.6(5) . . ?
C7 C8 C3 119.0(5) . . ?
C7 C8 C9 116.4(4) . . ?
O3 C3 C8 123.7(5) . . ?
O3 C3 C4 118.3(4) . . ?
C4 C3 C8 117.9(4) . . ?
N1 C9 C8 128.7(4) . . ?
N1 C9 H9 115.6 . . ?
C8 C9 H9 115.6 . . ?
C12 C13 Br1 119.7(3) . . ?
C12 C13 C14 121.5(5) . . ?
C14 C13 Br1 118.8(5) . . ?
C10 C15 H15 119.4 . . ?
C10 C15 C14 121.3(4) . . ?
C14 C15 H15 119.4 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.5(5) . . ?
C5 C4 H4 119.3 . . ?
C15 C10 N1 120.0(4) . . ?
C15 C10 C11 119.4(5) . . ?
C11 C10 N1 120.6(5) . . ?
C13 C12 H12 120.3 . . ?
C13 C12 C11 119.5(4) . . ?
C11 C12 H12 120.3 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.6(6) . . ?
C15 C14 H14 120.7 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.7(5) . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 178.5(6) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 C8 121.5(5) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 Rh1 173.3(6) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(5) . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 119.5(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -5.0(9) . . . . ?
Rh1 O3 C3 C4 175.6(4) . . . . ?
Rh1 N1 C9 C8 -8.8(8) . . . . ?
Rh1 N1 C10 C15 36.4(7) . . . . ?
Rh1 N1 C10 C11 -144.6(4) . . . . ?
Br1 C13 C12 C11 -179.1(4) . . . . ?
Br1 C13 C14 C15 179.0(4) . . . . ?
O3 C3 C4 C5 177.3(5) . . . . ?
N1 C10 C11 C12 179.5(5) . . . . ?
C8 C3 C4 C5 -2.1(9) . . . . ?
C8 C7 C6 C5 1.7(8) . . . . ?
C3 C8 C9 N1 5.7(10) . . . . ?
C3 C8 C7 C6 -3.0(8) . . . . ?
C3 C4 C5 C6 0.9(9) . . . . ?
C9 N1 C10 C15 -145.1(6) . . . . ?
C9 N1 C10 C11 33.9(7) . . . . ?
C9 C8 C3 O3 2.0(10) . . . . ?
C9 C8 C3 C4 -178.5(6) . . . . ?
C9 C8 C7 C6 178.5(6) . . . . ?
C13 C12 C11 C10 0.9(7) . . . . ?
C15 C10 C11 C12 -1.5(8) . . . . ?
C4 C5 C6 C7 -0.6(8) . . . . ?
C10 N1 C9 C8 172.7(6) . . . . ?
C10 C15 C14 C13 -0.8(9) . . . . ?
C12 C13 C14 C15 0.2(9) . . . . ?
C14 C13 C12 C11 -0.3(8) . . . . ?
C14 C15 C10 N1 -179.6(5) . . . . ?
C14 C15 C10 C11 1.4(9) . . . . ?
C7 C8 C3 O3 -176.3(5) . . . . ?
C7 C8 C3 C4 3.1(8) . . . . ?
C7 C8 C9 N1 -175.9(5) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.01700000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.773
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-01-HP-UW-5p71GPa
_database_code_depnum_ccdc_archive 'CCDC 2427955'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-02-28 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-01-HP-UW-5p71GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.341 Why?
RESPONSE: High-pressure data collection at the home source. Sample
 enclosed a in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.494(7)
_cell_length_b                   14.480(3)
_cell_length_c                   9.449(17)
_cell_angle_alpha                90
_cell_angle_beta                 103.54(14)
_cell_angle_gamma                90
_cell_volume                     1130(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    975
_cell_measurement_theta_min      2.7870
_cell_measurement_theta_max      25.0230

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.552
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    5.057
_shelx_estimated_absorpt_T_min   0.632
_shelx_estimated_absorpt_T_max   0.751
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_T_max  0.329
_exptl_absorpt_process_details   
'A numerical (Gaussian)absorption correction for both the crystal and high-pressure cell using Absorb program within CrysAlisPro (Rigaku Oxford Diffraction, version 171.43.100a).'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3174
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.813
_diffrn_reflns_theta_max         25.335
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.340
_diffrn_measured_fraction_theta_full 0.341
_diffrn_reflns_Laue_measured_fraction_max 0.340
_diffrn_reflns_Laue_measured_fraction_full 0.341
_diffrn_reflns_point_group_measured_fraction_max 0.340
_diffrn_reflns_point_group_measured_fraction_full 0.341
_reflns_number_total             703
_reflns_number_gt                446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1649P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         703
_refine_ls_number_parameters     190
_refine_ls_number_restraints     284
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2443
_refine_ls_wR_factor_gt          0.2006
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      0.895
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.4778(5) 0.45923(13) 0.6410(5) 0.0216(10) Uani 1 1 d D U . . .
Br1 Br 1.3355(6) 0.55277(16) 0.9632(6) 0.033(3) Uani 1 1 d D U . . .
O3 O 0.275(3) 0.5337(9) 0.596(3) 0.021(5) Uani 1 1 d D U . . .
N1 N 0.604(3) 0.5743(11) 0.738(4) 0.029(8) Uani 1 1 d D U . . .
O2 O 0.279(4) 0.3006(11) 0.507(4) 0.031(7) Uani 1 1 d D U . . .
C8 C 0.379(3) 0.6804(13) 0.680(5) 0.0207(13) Uani 1 1 d D U . . .
O1 O 0.726(3) 0.3165(10) 0.738(4) 0.031(7) Uani 1 1 d D U . . .
C9 C 0.542(4) 0.6543(14) 0.747(5) 0.0208(13) Uani 1 1 d D U . . .
H9 H 0.608405 0.698985 0.801487 0.025 Uiso 1 1 calc R U . . .
C3 C 0.255(3) 0.6221(11) 0.603(5) 0.0208(13) Uani 1 1 d D U . . .
C10 C 0.778(3) 0.5723(13) 0.782(3) 0.0195(12) Uani 1 1 d D U . . .
C15 C 0.871(3) 0.5139(15) 0.721(3) 0.0193(12) Uani 1 1 d D U . . .
H15 H 0.822145 0.478603 0.640832 0.023 Uiso 1 1 calc R U . . .
C13 C 1.109(2) 0.5623(14) 0.891(4) 0.0191(12) Uani 1 1 d D U . . .
C11 C 0.854(3) 0.6278(12) 0.897(3) 0.0195(12) Uani 1 1 d D U . . .
H11 H 0.792712 0.668596 0.938087 0.023 Uiso 1 1 calc R U . . .
C14 C 1.036(3) 0.5060(14) 0.776(4) 0.0192(12) Uani 1 1 d D U . . .
H14 H 1.096826 0.463743 0.737229 0.023 Uiso 1 1 calc R U . . .
C12 C 1.020(3) 0.6235(13) 0.952(3) 0.0195(13) Uani 1 1 d D U . . .
H12 H 1.070193 0.661363 1.029016 0.023 Uiso 1 1 calc R U . . .
C7 C 0.344(4) 0.7740(12) 0.703(4) 0.0207(13) Uani 1 1 d D U . . .
H7 H 0.425652 0.812766 0.753076 0.025 Uiso 1 1 calc R U . . .
C4 C 0.100(3) 0.6584(13) 0.551(5) 0.0208(13) Uani 1 1 d D U . . .
H4 H 0.016620 0.621292 0.499584 0.025 Uiso 1 1 calc R U . . .
C2 C 0.358(5) 0.3582(13) 0.555(6) 0.022(7) Uani 1 1 d D U . . .
C1 C 0.639(4) 0.3745(14) 0.698(6) 0.022(6) Uani 1 1 d D U . . .
C5 C 0.071(4) 0.7488(12) 0.578(4) 0.0208(13) Uani 1 1 d D U . . .
H5 H -0.032910 0.772084 0.544062 0.025 Uiso 1 1 calc R U . . .
C6 C 0.192(3) 0.8076(13) 0.653(4) 0.0208(13) Uani 1 1 d D U . . .
H6 H 0.168303 0.868970 0.668997 0.025 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.825(17) . ?
Rh1 C2 1.855(15) . ?
Rh1 O3 1.989(17) . ?
Rh1 N1 2.077(14) . ?
Rh1 Rh1 3.018(12) 3_666 ?
Br1 C13 1.887(17) . ?
O3 C3 1.295(16) . ?
N1 C9 1.284(19) . ?
N1 C10 1.44(2) . ?
O2 C2 1.099(16) . ?
C8 C3 1.414(18) . ?
C8 C7 1.415(18) . ?
C8 C9 1.43(2) . ?
O1 C1 1.123(16) . ?
C9 H9 0.9300 . ?
C3 C4 1.396(19) . ?
C10 C15 1.37(2) . ?
C10 C11 1.385(18) . ?
C15 C14 1.379(19) . ?
C15 H15 0.9300 . ?
C13 C12 1.38(2) . ?
C13 C14 1.384(19) . ?
C11 C12 1.384(19) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C7 C6 1.359(19) . ?
C7 H7 0.9300 . ?
C4 C5 1.365(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(18) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 C2 84.0(12) . . ?
C1 Rh1 O3 168.3(19) . . ?
C2 Rh1 O3 88.7(12) . . ?
C1 Rh1 N1 97.6(9) . . ?
C2 Rh1 N1 178(2) . . ?
O3 Rh1 N1 89.5(7) . . ?
C1 Rh1 Rh1 107(2) . 3_666 ?
C2 Rh1 Rh1 95.3(19) . 3_666 ?
O3 Rh1 Rh1 83.1(11) . 3_666 ?
N1 Rh1 Rh1 85.3(13) . 3_666 ?
C3 O3 Rh1 130.2(17) . . ?
C9 N1 C10 114.2(18) . . ?
C9 N1 Rh1 125.0(15) . . ?
C10 N1 Rh1 120.1(15) . . ?
C3 C8 C7 119.6(17) . . ?
C3 C8 C9 126.7(18) . . ?
C7 C8 C9 113.7(17) . . ?
N1 C9 C8 125(2) . . ?
N1 C9 H9 117.3 . . ?
C8 C9 H9 117.3 . . ?
O3 C3 C4 118.8(17) . . ?
O3 C3 C8 121.6(17) . . ?
C4 C3 C8 119.0(16) . . ?
C15 C10 C11 118.5(18) . . ?
C15 C10 N1 123(2) . . ?
C11 C10 N1 118(2) . . ?
C10 C15 C14 121.9(19) . . ?
C10 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C12 C13 C14 121.2(17) . . ?
C12 C13 Br1 120.8(15) . . ?
C14 C13 Br1 118.1(17) . . ?
C12 C11 C10 121.0(19) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C15 C14 C13 118(2) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C13 C12 C11 119.0(18) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C6 C7 C8 120.4(17) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C5 C4 C3 119.4(17) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
O2 C2 Rh1 175(5) . . ?
O1 C1 Rh1 173(4) . . ?
C4 C5 C6 122.6(19) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C7 C6 C5 119.0(18) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C9 C8 165(5) . . . . ?
Rh1 N1 C9 C8 -6(7) . . . . ?
C3 C8 C9 N1 5(8) . . . . ?
C7 C8 C9 N1 -178(5) . . . . ?
Rh1 O3 C3 C4 174(3) . . . . ?
Rh1 O3 C3 C8 -16(7) . . . . ?
C7 C8 C3 O3 -171(4) . . . . ?
C9 C8 C3 O3 6(7) . . . . ?
C7 C8 C3 C4 0(6) . . . . ?
C9 C8 C3 C4 177(5) . . . . ?
C9 N1 C10 C15 -148(4) . . . . ?
Rh1 N1 C10 C15 23(4) . . . . ?
C9 N1 C10 C11 37(5) . . . . ?
Rh1 N1 C10 C11 -152(2) . . . . ?
C11 C10 C15 C14 3(3) . . . . ?
N1 C10 C15 C14 -172(3) . . . . ?
C15 C10 C11 C12 -1(2) . . . . ?
N1 C10 C11 C12 175(2) . . . . ?
C10 C15 C14 C13 -3(4) . . . . ?
C12 C13 C14 C15 1(4) . . . . ?
Br1 C13 C14 C15 -179(2) . . . . ?
C14 C13 C12 C11 0(3) . . . . ?
Br1 C13 C12 C11 -179.4(16) . . . . ?
C10 C11 C12 C13 -0.5(18) . . . . ?
C3 C8 C7 C6 1(5) . . . . ?
C9 C8 C7 C6 -176(4) . . . . ?
O3 C3 C4 C5 170(4) . . . . ?
C8 C3 C4 C5 -1(6) . . . . ?
C3 C4 C5 C6 1(5) . . . . ?
C8 C7 C6 C5 -1(3) . . . . ?
C4 C5 C6 C7 0(3) . . . . ?

_refine_diff_density_max         1.718
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.211



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-20-HP-ESRF-10p45GPa
_database_code_depnum_ccdc_archive 'CCDC 2427949'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-20-HP-ESRF-10p45GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.443 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.3863(7)
_cell_length_b                   14.0446(12)
_cell_length_c                   9.0132(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.313(9)
_cell_angle_gamma                90
_cell_volume                     1037.16(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    635
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.7200
_cell_measurement_theta_min      2.1420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.780
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.443
_diffrn_reflns_Laue_measured_fraction_max 0.379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2257
_diffrn_reflns_point_group_measured_fraction_full 0.443
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.788
_diffrn_reflns_theta_min         2.138
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.443
_diffrn_measured_fraction_theta_max 0.379
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0291059000
_diffrn_orient_matrix_UB_12      0.0167696000
_diffrn_orient_matrix_UB_13      -0.0203738000
_diffrn_orient_matrix_UB_21      -0.0282314000
_diffrn_orient_matrix_UB_22      -0.0064572000
_diffrn_orient_matrix_UB_23      -0.0416966000
_diffrn_orient_matrix_UB_31      -0.0291386000
_diffrn_orient_matrix_UB_32      0.0229853000
_diffrn_orient_matrix_UB_33      0.0030471000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1219
_reflns_number_total             1369
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1369
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0752P)²+6.6422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1416
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47881(10) 0.45630(5) 0.63853(8) 0.0348(3) Uani 1 1 d D U . . .
Br1 Br 1.33812(12) 0.55333(6) 0.97031(10) 0.0352(3) Uani 1 1 d D U . . .
O3 O 0.2710(9) 0.5309(5) 0.5935(8) 0.0394(17) Uani 1 1 d D U . . .
N1 N 0.6092(9) 0.5748(5) 0.7297(8) 0.0329(14) Uani 1 1 d D U . . .
O2 O 0.2746(12) 0.2957(6) 0.4945(9) 0.051(3) Uani 1 1 d D U . . .
C8 C 0.3726(11) 0.6817(6) 0.6871(10) 0.0349(11) Uani 1 1 d D U . . .
C3 C 0.2489(11) 0.6193(6) 0.6122(10) 0.0348(11) Uani 1 1 d D U . . .
C9 C 0.5394(11) 0.6546(6) 0.7450(10) 0.034(2) Uani 1 1 d D U . . .
H9 H 0.605578 0.700847 0.800840 0.041 Uiso 1 1 calc R U . . .
O1 O 0.7356(11) 0.3130(6) 0.7359(9) 0.051(3) Uani 1 1 d D U . . .
C13 C 1.1114(11) 0.5617(6) 0.8969(10) 0.0363(9) Uani 1 1 d D U . . .
C15 C 0.8764(11) 0.5108(7) 0.7218(10) 0.0362(9) Uani 1 1 d D U . . .
H15 H 0.826344 0.472742 0.640670 0.043 Uiso 1 1 calc R U . . .
C4 C 0.0925(12) 0.6577(7) 0.5584(10) 0.0352(11) Uani 1 1 d D U . . .
H4 H 0.008182 0.618728 0.508694 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7835(10) 0.5722(7) 0.7851(9) 0.0363(9) Uani 1 1 d D U . . .
C12 C 1.0239(11) 0.6250(6) 0.9598(9) 0.0367(9) Uani 1 1 d D U . . .
H12 H 1.074563 0.663873 1.039553 0.044 Uiso 1 1 calc R U . . .
C14 C 1.0432(11) 0.5039(7) 0.7757(10) 0.0362(10) Uani 1 1 d D U . . .
H14 H 1.106659 0.462369 0.732401 0.043 Uiso 1 1 calc R U . . .
C11 C 0.8560(11) 0.6307(6) 0.9025(9) 0.0367(9) Uani 1 1 d D U . . .
H11 H 0.793344 0.673929 0.943557 0.044 Uiso 1 1 calc R U . . .
C2 C 0.3531(13) 0.3536(7) 0.5504(11) 0.039(3) Uani 1 1 d D U . . .
C7 C 0.3364(11) 0.7755(6) 0.7094(9) 0.0354(11) Uani 1 1 d D U . . .
H7 H 0.417140 0.814937 0.763910 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6436(12) 0.3706(6) 0.6964(10) 0.035(2) Uani 1 1 d D U . . .
C5 C 0.0640(12) 0.7510(7) 0.5786(10) 0.0357(11) Uani 1 1 d D U . . .
H5 H -0.040151 0.775020 0.541034 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1836(11) 0.8120(7) 0.6528(9) 0.0358(11) Uani 1 1 d D U . . .
H6 H 0.161403 0.876174 0.664155 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.8718(17) 3_666 ?
Rh1 O3 1.999(7) . ?
Rh1 N1 2.064(7) . ?
Rh1 C2 1.862(8) . ?
Rh1 C1 1.823(8) . ?
Br1 C13 1.879(8) . ?
O3 C3 1.273(10) . ?
N1 C9 1.284(11) . ?
N1 C10 1.441(10) . ?
O2 C2 1.099(10) . ?
C8 C3 1.414(10) . ?
C8 C9 1.436(11) . ?
C8 C7 1.376(12) . ?
C3 C4 1.405(11) . ?
C9 H9 0.9300 . ?
O1 C1 1.123(10) . ?
C13 C12 1.352(13) . ?
C13 C14 1.383(10) . ?
C15 H15 0.9300 . ?
C15 C10 1.366(13) . ?
C15 C14 1.383(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.352(12) . ?
C10 C11 1.375(10) . ?
C12 H12 0.9300 . ?
C12 C11 1.395(10) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.374(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.378(11) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.2(3) . 3_666 ?
O3 Rh1 N1 91.3(3) . . ?
N1 Rh1 Rh1 81.3(2) . 3_666 ?
C2 Rh1 Rh1 97.1(3) . 3_666 ?
C2 Rh1 O3 86.0(4) . . ?
C2 Rh1 N1 177.0(3) . . ?
C1 Rh1 Rh1 107.7(4) . 3_666 ?
C1 Rh1 O3 168.2(5) . . ?
C1 Rh1 N1 96.5(3) . . ?
C1 Rh1 C2 86.3(4) . . ?
C3 O3 Rh1 129.1(6) . . ?
C9 N1 Rh1 122.1(6) . . ?
C9 N1 C10 115.9(7) . . ?
C10 N1 Rh1 122.0(6) . . ?
C3 C8 C9 124.6(8) . . ?
C7 C8 C3 120.0(7) . . ?
C7 C8 C9 115.4(7) . . ?
O3 C3 C8 123.7(8) . . ?
O3 C3 C4 118.7(7) . . ?
C4 C3 C8 117.6(8) . . ?
N1 C9 C8 128.5(8) . . ?
N1 C9 H9 115.7 . . ?
C8 C9 H9 115.7 . . ?
C12 C13 Br1 119.5(5) . . ?
C12 C13 C14 123.2(8) . . ?
C14 C13 Br1 117.3(8) . . ?
C10 C15 H15 119.3 . . ?
C10 C15 C14 121.4(8) . . ?
C14 C15 H15 119.3 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.3(7) . . ?
C5 C4 H4 119.9 . . ?
C15 C10 N1 119.9(7) . . ?
C15 C10 C11 120.0(8) . . ?
C11 C10 N1 120.1(9) . . ?
C13 C12 H12 120.7 . . ?
C13 C12 C11 118.5(7) . . ?
C11 C12 H12 120.7 . . ?
C13 C14 C15 117.0(9) . . ?
C13 C14 H14 121.5 . . ?
C15 C14 H14 121.5 . . ?
C10 C11 C12 119.8(9) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 176.9(9) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.4(8) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 174.1(11) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.5(8) . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 118.2(8) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -7.2(15) . . . . ?
Rh1 O3 C3 C4 174.0(8) . . . . ?
Rh1 N1 C9 C8 -9.3(15) . . . . ?
Rh1 N1 C10 C15 29.7(13) . . . . ?
Rh1 N1 C10 C11 -149.6(7) . . . . ?
Br1 C13 C12 C11 179.3(6) . . . . ?
Br1 C13 C14 C15 -179.7(7) . . . . ?
O3 C3 C4 C5 178.9(9) . . . . ?
N1 C10 C11 C12 177.3(8) . . . . ?
C8 C3 C4 C5 0.1(16) . . . . ?
C8 C7 C6 C5 3.0(13) . . . . ?
C3 C8 C9 N1 6.3(18) . . . . ?
C3 C8 C7 C6 -3.7(15) . . . . ?
C3 C4 C5 C6 -0.7(15) . . . . ?
C9 N1 C10 C15 -152.4(10) . . . . ?
C9 N1 C10 C11 28.3(12) . . . . ?
C9 C8 C3 O3 3.0(17) . . . . ?
C9 C8 C3 C4 -178.2(10) . . . . ?
C9 C8 C7 C6 176.6(9) . . . . ?
C13 C12 C11 C10 0.3(11) . . . . ?
C15 C10 C11 C12 -2.0(12) . . . . ?
C4 C5 C6 C7 -0.8(13) . . . . ?
C10 N1 C9 C8 172.8(10) . . . . ?
C10 C15 C14 C13 0.3(16) . . . . ?
C12 C13 C14 C15 -2.1(16) . . . . ?
C14 C13 C12 C11 1.7(15) . . . . ?
C14 C15 C10 N1 -177.6(9) . . . . ?
C14 C15 C10 C11 1.7(15) . . . . ?
C7 C8 C3 O3 -176.7(10) . . . . ?
C7 C8 C3 C4 2.1(15) . . . . ?
C7 C8 C9 N1 -174.0(10) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.02010000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Rh-4-Br-12-HP-ESRF-5p60GPa
_database_code_depnum_ccdc_archive 'CCDC 2427948'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2025-05-22 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_Rh-4-Br-12-HP-ESRF-5p60GPa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.456 Why?
RESPONSE: High-pressure data collection at synchrotron. Sample enclosed
 in diamond-anvil cell, thus limited coverage.
;
# end Validation Reply Form

_audit_creation_date             2025-02-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 Br N O3 Rh'
_chemical_formula_sum            'C15 H9 Br N O3 Rh'
_chemical_formula_weight         434.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H9 N1 O3 Rh1 Br1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.2857 0.9486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0016 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -0.3111 2.3481 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5648(5)
_cell_length_b                   14.2276(7)
_cell_length_c                   9.5562(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.001(4)
_cell_angle_gamma                90
_cell_volume                     1129.89(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1019
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.4210
_cell_measurement_theta_min      2.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Piezochromic
_exptl_crystal_density_diffrn    2.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.456
_diffrn_reflns_Laue_measured_fraction_max 0.385
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2526
_diffrn_reflns_point_group_measured_fraction_full 0.456
_diffrn_reflns_point_group_measured_fraction_max 0.385
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         17.798
_diffrn_reflns_theta_min         2.080
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.456
_diffrn_measured_fraction_theta_max 0.385
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0284033000
_diffrn_orient_matrix_UB_12      0.0162362000
_diffrn_orient_matrix_UB_13      0.0191361000
_diffrn_orient_matrix_UB_21      0.0271803000
_diffrn_orient_matrix_UB_22      -0.0076024000
_diffrn_orient_matrix_UB_23      0.0398021000
_diffrn_orient_matrix_UB_31      0.0297218000
_diffrn_orient_matrix_UB_32      0.0225022000
_diffrn_orient_matrix_UB_33      -0.0003900000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1389
_reflns_number_total             1513
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1513
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+2.5582P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0959
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.367 with sigma of 0.02
 C6-C5
 1.398 with sigma of 0.02
 C5-C4
 1.369 with sigma of 0.02
 C4-C3
 1.412 with sigma of 0.02
 C3-C8
 1.412 with sigma of 0.02
 C8-C7
 1.416 with sigma of 0.02
 C8-C9
 1.438 with sigma of 0.02
 C9-N1
 1.29 with sigma of 0.02
 N1-Rh1
 2.079 with sigma of 0.02
 Rh1-O3
 2.0145 with sigma of 0.02
 O3-C3
 1.306 with sigma of 0.02
 Rh1-C1
 1.836 with sigma of 0.02
 Rh1-C2
 1.878 with sigma of 0.02
 C1-O1
 1.13 with sigma of 0.02
 C2-O2
 1.108 with sigma of 0.02
 N1-C10
 1.448 with sigma of 0.02
 C10-C11
 1.381 with sigma of 0.02
 C11-C12
 1.392 with sigma of 0.02
 C12-C13
 1.374 with sigma of 0.02
 C13-C14
 1.375 with sigma of 0.02
 C14-C15
 1.395 with sigma of 0.02
 C15-C10
 1.387 with sigma of 0.02
 C13-Br1
 1.9 with sigma of 0.02
 C7-C5
 2.382 with sigma of 0.04
 C7-C3
 2.441 with sigma of 0.04
 C6-C8
 2.429 with sigma of 0.04
 C6-C4
 2.408 with sigma of 0.04
 C5-C3
 2.425 with sigma of 0.04
 C4-C8
 2.418 with sigma of 0.04
 C10-C12
 2.406 with sigma of 0.04
 C10-C14
 2.409 with sigma of 0.04
 C11-C15
 2.396 with sigma of 0.04
 C11-C13
 2.384 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.04
 C13-C15
 2.389 with sigma of 0.04
3. Restrained planarity
 C7, C6, C5, C4, C3, C8
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, Br1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim C7
\\sim C8 \\sim C8 \\sim C3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C10 \\sim C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim
C14 \\sim C15 \\sim C15 \\sim C10: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C4(H4), C12(H12), C14(H14), C11(H11), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47955(6) 0.45744(3) 0.63765(4) 0.02569(17) Uani 1 1 d D U . . .
Br1 Br 1.33365(7) 0.55465(4) 0.96500(5) 0.0285(2) Uani 1 1 d D U . . .
O3 O 0.2767(6) 0.5329(3) 0.5905(4) 0.0307(10) Uani 1 1 d D U . . .
N1 N 0.6095(6) 0.5740(3) 0.7304(4) 0.0252(9) Uani 1 1 d D U . . .
O2 O 0.2828(7) 0.2956(3) 0.4974(5) 0.0424(16) Uani 1 1 d D U . . .
C8 C 0.3782(7) 0.6815(4) 0.6875(5) 0.0265(7) Uani 1 1 d D U . . .
C3 C 0.2555(7) 0.6216(4) 0.6120(5) 0.0266(7) Uani 1 1 d D U . . .
C9 C 0.5422(7) 0.6530(4) 0.7442(5) 0.0266(12) Uani 1 1 d D U . . .
H9 H 0.609015 0.698114 0.798503 0.032 Uiso 1 1 calc R U . . .
O1 O 0.7317(7) 0.3150(3) 0.7359(5) 0.0450(16) Uani 1 1 d D U . . .
C13 C 1.1094(7) 0.5630(4) 0.8925(5) 0.0269(6) Uani 1 1 d D U . . .
C15 C 0.8729(7) 0.5174(4) 0.7184(5) 0.0271(6) Uani 1 1 d D U . . .
H15 H 0.823786 0.483991 0.635849 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1009(8) 0.6600(4) 0.5593(5) 0.0279(7) Uani 1 1 d D U . . .
H4 H 0.018638 0.621966 0.507550 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7805(7) 0.5709(4) 0.7856(5) 0.0271(6) Uani 1 1 d D U . . .
C12 C 1.0209(7) 0.6179(4) 0.9607(5) 0.0275(6) Uani 1 1 d D U . . .
H12 H 1.070968 0.651671 1.042546 0.033 Uiso 1 1 calc R U . . .
C14 C 1.0377(7) 0.5117(4) 0.7704(5) 0.0270(6) Uani 1 1 d D U . . .
H14 H 1.099223 0.474309 0.724634 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8553(7) 0.6231(4) 0.9074(5) 0.0277(6) Uani 1 1 d D U . . .
H11 H 0.794158 0.661218 0.952690 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3553(8) 0.3545(4) 0.5508(6) 0.0296(15) Uani 1 1 d D U . . .
C7 C 0.3409(8) 0.7758(4) 0.7115(5) 0.0276(7) Uani 1 1 d D U . . .
H7 H 0.420946 0.814781 0.764386 0.033 Uiso 1 1 calc R U . . .
C1 C 0.6420(8) 0.3730(4) 0.6970(6) 0.0307(14) Uani 1 1 d D U . . .
C5 C 0.0699(8) 0.7515(4) 0.5825(5) 0.0291(7) Uani 1 1 d D U . . .
H5 H -0.033441 0.775014 0.546800 0.035 Uiso 1 1 calc R U . . .
C6 C 0.1901(8) 0.8109(4) 0.6588(5) 0.0288(7) Uani 1 1 d D U . . .
H6 H 0.167711 0.873594 0.673629 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.9927(9) 3_666 ?
Rh1 O3 1.999(4) . ?
Rh1 N1 2.073(4) . ?
Rh1 C2 1.881(5) . ?
Rh1 C1 1.821(6) . ?
Br1 C13 1.881(6) . ?
O3 C3 1.298(6) . ?
N1 C9 1.285(7) . ?
N1 C10 1.432(7) . ?
O2 C2 1.093(6) . ?
C8 C3 1.409(7) . ?
C8 C9 1.436(8) . ?
C8 C7 1.410(7) . ?
C3 C4 1.407(8) . ?
C9 H9 0.9300 . ?
O1 C1 1.128(7) . ?
C13 C12 1.359(9) . ?
C13 C14 1.387(6) . ?
C15 H15 0.9300 . ?
C15 C10 1.365(9) . ?
C15 C14 1.380(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.359(8) . ?
C10 C11 1.399(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.388(7) . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.363(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(7) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 Rh1 82.23(15) . 3_666 ?
O3 Rh1 N1 90.81(18) . . ?
N1 Rh1 Rh1 83.51(13) . 3_666 ?
C2 Rh1 Rh1 95.80(19) . 3_666 ?
C2 Rh1 O3 87.2(2) . . ?
C2 Rh1 N1 177.9(2) . . ?
C1 Rh1 Rh1 107.3(2) . 3_666 ?
C1 Rh1 O3 168.8(3) . . ?
C1 Rh1 N1 96.0(2) . . ?
C1 Rh1 C2 86.1(3) . . ?
C3 O3 Rh1 129.3(4) . . ?
C9 N1 Rh1 122.4(4) . . ?
C9 N1 C10 115.7(4) . . ?
C10 N1 Rh1 121.9(4) . . ?
C3 C8 C9 124.2(5) . . ?
C3 C8 C7 119.3(5) . . ?
C7 C8 C9 116.5(5) . . ?
O3 C3 C8 123.6(5) . . ?
O3 C3 C4 118.4(5) . . ?
C4 C3 C8 118.0(5) . . ?
N1 C9 C8 129.1(5) . . ?
N1 C9 H9 115.4 . . ?
C8 C9 H9 115.4 . . ?
C12 C13 Br1 119.9(3) . . ?
C12 C13 C14 121.3(5) . . ?
C14 C13 Br1 118.8(5) . . ?
C10 C15 H15 119.3 . . ?
C10 C15 C14 121.5(5) . . ?
C14 C15 H15 119.3 . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.2(5) . . ?
C5 C4 H4 119.4 . . ?
C15 C10 N1 120.1(4) . . ?
C15 C10 C11 119.1(5) . . ?
C11 C10 N1 120.8(6) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.6(6) . . ?
C15 C14 H14 120.7 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.9(6) . . ?
C12 C11 H11 120.1 . . ?
O2 C2 Rh1 178.5(6) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.3(5) . . ?
C6 C7 H7 119.3 . . ?
O1 C1 Rh1 173.4(7) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(5) . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.0(5) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 O3 C3 C8 -5.6(9) . . . . ?
Rh1 O3 C3 C4 175.5(5) . . . . ?
Rh1 N1 C9 C8 -8.3(9) . . . . ?
Rh1 N1 C10 C15 35.3(8) . . . . ?
Rh1 N1 C10 C11 -145.4(4) . . . . ?
Br1 C13 C12 C11 -179.4(4) . . . . ?
Br1 C13 C14 C15 179.4(4) . . . . ?
O3 C3 C4 C5 177.8(6) . . . . ?
N1 C10 C11 C12 178.9(5) . . . . ?
C8 C3 C4 C5 -1.2(10) . . . . ?
C8 C7 C6 C5 1.4(9) . . . . ?
C3 C8 C9 N1 5.0(11) . . . . ?
C3 C8 C7 C6 -2.3(9) . . . . ?
C3 C4 C5 C6 0.3(9) . . . . ?
C9 N1 C10 C15 -145.8(6) . . . . ?
C9 N1 C10 C11 33.5(8) . . . . ?
C9 C8 C3 O3 2.8(10) . . . . ?
C9 C8 C3 C4 -178.3(6) . . . . ?
C9 C8 C7 C6 178.1(6) . . . . ?
C13 C12 C11 C10 1.0(8) . . . . ?
C15 C10 C11 C12 -1.8(8) . . . . ?
C4 C5 C6 C7 -0.4(9) . . . . ?
C10 N1 C9 C8 172.8(6) . . . . ?
C10 C15 C14 C13 -1.0(9) . . . . ?
C12 C13 C14 C15 0.1(9) . . . . ?
C14 C13 C12 C11 -0.2(9) . . . . ?
C14 C15 C10 N1 -178.9(5) . . . . ?
C14 C15 C10 C11 1.8(9) . . . . ?
C7 C8 C3 O3 -176.8(6) . . . . ?
C7 C8 C3 C4 2.2(9) . . . . ?
C7 C8 C9 N1 -175.4(6) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . -0.02421000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.749
