# Supplementary Information (SI) for Dalton Transactions.
# 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_rmk_326_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2403969'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-06-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H32 Fe2 Li2 N6 O8'
_chemical_formula_sum            'C22 H32 Fe2 Li2 N6 O8'
_chemical_formula_weight         634.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Fe N Li N'
_chemical_oxdiff_usercomment     'THF evap'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6531(15)
_cell_length_b                   9.7961(15)
_cell_length_c                   10.6609(13)
_cell_angle_alpha                116.394(14)
_cell_angle_beta                 108.038(12)
_cell_angle_gamma                97.046(13)
_cell_volume                     817.6(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2517
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.6200
_cell_measurement_theta_min      3.9980
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.787
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.061
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8226
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.813
_diffrn_reflns_theta_min         3.466
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  28.00   1.00  110.00    --  -11.14 -99.00 -90.00   33
  2  ω    -10.00  81.00   1.00  110.00    --   11.46  57.00-180.00   91
  3  ω    -10.00  84.00   1.00  110.00    --   11.46  37.00 -30.00   94
  4  ω    -61.00  40.00   1.00  110.00    --   11.46 -57.00  30.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0093156000
_diffrn_orient_matrix_UB_12      -0.0571976000
_diffrn_orient_matrix_UB_13      -0.0747438000
_diffrn_orient_matrix_UB_21      0.0569783000
_diffrn_orient_matrix_UB_22      -0.0284026000
_diffrn_orient_matrix_UB_23      0.0321520000
_diffrn_orient_matrix_UB_31      -0.0570272000
_diffrn_orient_matrix_UB_32      -0.0559437000
_diffrn_orient_matrix_UB_33      -0.0031099000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5222
_reflns_number_total             8226
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         8226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0644
_refine_ls_restrained_S_all      0.944
_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)+(0.1144P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1797
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.70212
 0.29788
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe1 Fe 0.19323(7) 0.51991(8) 0.37552(8) 0.0289(2) Uani 1 1 d . . . . .
N1 N 0.4140(4) 0.8332(4) 0.4653(4) 0.0305(9) Uani 1 1 d . . . . .
O4 O 0.2686(4) 0.3627(5) 0.1104(4) 0.0567(11) Uani 1 1 d . . . . .
N3 N 0.5916(4) 0.8486(5) 0.2260(4) 0.0323(9) Uani 1 1 d . . . . .
N2 N 0.2941(4) 0.8973(5) 0.1626(5) 0.0383(10) Uani 1 1 d . . . . .
O1 O -0.0089(4) 0.2137(4) 0.2874(5) 0.0618(12) Uani 1 1 d . . . . .
O3 O -0.0552(5) 0.6627(6) 0.3406(6) 0.0780(14) Uani 1 1 d . . . . .
O2 O 0.3736(5) 0.5817(5) 0.6836(5) 0.0742(14) Uani 1 1 d . . . . .
C5 C 0.3312(5) 0.7150(5) 0.4316(5) 0.0240(10) Uani 1 1 d . . . . .
C1 C 0.0687(5) 0.3339(6) 0.3223(6) 0.0390(12) Uani 1 1 d . . . . .
C3 C 0.0397(6) 0.6069(7) 0.3543(6) 0.0446(14) Uani 1 1 d . . . . .
C4 C 0.2409(5) 0.4228(5) 0.2150(6) 0.0335(11) Uani 1 1 d . . . . .
C2 C 0.3040(5) 0.5554(6) 0.5642(6) 0.0408(13) Uani 1 1 d . . . . .
Li1 Li 0.4717(8) 0.9404(9) 0.3548(8) 0.0282(17) Uani 1 1 d . . . . .
C10 C 0.5932(6) 0.6924(7) 0.2068(7) 0.0523(15) Uani 1 1 d . . . . .
H10A H 0.653012 0.704919 0.303999 0.079 Uiso 1 1 calc R U . . .
H10B H 0.637299 0.642151 0.135395 0.079 Uiso 1 1 calc R U . . .
H10C H 0.490413 0.627055 0.168273 0.079 Uiso 1 1 calc R U . . .
C11 C 0.7510(6) 0.9465(7) 0.2868(7) 0.0623(18) Uani 1 1 d . . . . .
H11A H 0.752205 1.048927 0.296491 0.093 Uiso 1 1 calc R U . . .
H11B H 0.796531 0.893228 0.217864 0.093 Uiso 1 1 calc R U . . .
H11C H 0.807959 0.961128 0.385695 0.093 Uiso 1 1 calc R U . . .
C9 C 0.5007(7) 0.8357(9) 0.0798(6) 0.0620(18) Uani 1 1 d . . . . .
H9A H 0.531398 0.937816 0.086960 0.074 Uiso 1 1 calc R U . . .
H9B H 0.521824 0.756877 -0.001377 0.074 Uiso 1 1 calc R U . . .
C7 C 0.2953(7) 1.0470(8) 0.1651(8) 0.0677(19) Uani 1 1 d . . . . .
H7A H 0.265897 1.113469 0.244214 0.102 Uiso 1 1 calc R U . . .
H7B H 0.224511 1.025277 0.067491 0.102 Uiso 1 1 calc R U . . .
H7C H 0.396355 1.101231 0.185158 0.102 Uiso 1 1 calc R U . . .
C8 C 0.3357(7) 0.7892(9) 0.0400(6) 0.0652(19) Uani 1 1 d . . . . .
H8A H 0.302630 0.681114 0.019679 0.078 Uiso 1 1 calc R U . . .
H8B H 0.281599 0.789216 -0.053361 0.078 Uiso 1 1 calc R U . . .
C6 C 0.1416(6) 0.8182(8) 0.1387(7) 0.069(2) Uani 1 1 d . . . . .
H6A H 0.140105 0.718226 0.134927 0.104 Uiso 1 1 calc R U . . .
H6B H 0.067399 0.798784 0.043664 0.104 Uiso 1 1 calc R U . . .
H6C H 0.117407 0.885598 0.221771 0.104 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
Fe1 C5 1.911(4) . ?
Fe1 C1 1.791(5) . ?
Fe1 C3 1.802(6) . ?
Fe1 C4 1.787(5) . ?
Fe1 C2 1.807(5) . ?
N1 C5 1.155(5) . ?
N1 Li1 2.041(8) . ?
N1 Li1 2.031(8) 2_676 ?
O4 C4 1.140(6) . ?
N3 Li1 2.043(9) . ?
N3 C10 1.453(7) . ?
N3 C11 1.474(6) . ?
N3 C9 1.471(6) . ?
N2 Li1 2.048(8) . ?
N2 C7 1.454(7) . ?
N2 C8 1.479(7) . ?
N2 C6 1.464(7) . ?
O1 C1 1.143(5) . ?
O3 C3 1.128(6) . ?
O2 C2 1.129(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.468(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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 Fe1 C5 178.1(2) . . ?
C1 Fe1 C3 92.8(2) . . ?
C1 Fe1 C2 92.1(2) . . ?
C3 Fe1 C5 89.0(2) . . ?
C3 Fe1 C2 117.8(3) . . ?
C4 Fe1 C5 87.53(19) . . ?
C4 Fe1 C1 91.2(2) . . ?
C4 Fe1 C3 118.3(2) . . ?
C4 Fe1 C2 123.5(2) . . ?
C2 Fe1 C5 87.43(18) . . ?
C5 N1 Li1 141.2(4) . 2_676 ?
C5 N1 Li1 137.0(4) . . ?
Li1 N1 Li1 79.9(3) 2_676 . ?
C10 N3 Li1 108.8(4) . . ?
C10 N3 C11 108.1(4) . . ?
C10 N3 C9 111.5(4) . . ?
C11 N3 Li1 116.2(4) . . ?
C9 N3 Li1 102.4(4) . . ?
C9 N3 C11 109.8(5) . . ?
C7 N2 Li1 109.2(4) . . ?
C7 N2 C8 111.5(5) . . ?
C7 N2 C6 109.4(5) . . ?
C8 N2 Li1 101.1(4) . . ?
C6 N2 Li1 115.9(4) . . ?
C6 N2 C8 109.5(5) . . ?
N1 C5 Fe1 179.7(4) . . ?
O1 C1 Fe1 178.7(5) . . ?
O3 C3 Fe1 179.0(5) . . ?
O4 C4 Fe1 177.9(5) . . ?
O2 C2 Fe1 178.2(5) . . ?
N1 Li1 N1 100.1(3) 2_676 . ?
N1 Li1 N3 113.3(4) 2_676 . ?
N1 Li1 N3 119.6(4) . . ?
N1 Li1 N2 120.9(4) 2_676 . ?
N1 Li1 N2 114.4(3) . . ?
N3 Li1 N2 89.9(3) . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C9 H9A 109.1 . . ?
N3 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C8 C9 N3 112.3(5) . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.0 . . ?
N2 C8 H8B 109.0 . . ?
C9 C8 N2 112.8(5) . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
N3 C9 C8 N2 55.0(8) . . . . ?
Li1 N3 C9 C8 -36.5(6) . . . . ?
Li1 N2 C8 C9 -39.1(6) . . . . ?
C10 N3 C9 C8 79.7(6) . . . . ?
C11 N3 C9 C8 -160.5(5) . . . . ?
C7 N2 C8 C9 76.9(6) . . . . ?
C6 N2 C8 C9 -161.9(5) . . . . ?

_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.758
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.70212 3979 2965 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.29788 3871 2965 nmt 0.9508 -0.1175 -0.0834 0.1075 1.0379 0.0605 0.0202
-0.0136 1.0012

_twin_special_details            
;
Component 2 rotated by 6.7489° 
around [-0.30 -0.45 0.84] (reciprocal) or [-0.18 -0.26 0.95] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_rmk_365_b_scale
_database_code_depnum_ccdc_archive 'CCDC 2403981'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H5 N O5 W'
_chemical_formula_sum            'C12 H5 N O5 W'
_chemical_formula_weight         427.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12H5W1O5N1 '
_chemical_oxdiff_usercomment     'Et2O/hexane at 0 deg'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.33250(10)
_cell_length_b                   13.4583(2)
_cell_length_c                   9.66530(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.7130(10)
_cell_angle_gamma                90
_cell_volume                     1320.61(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6395
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.5280
_cell_measurement_theta_min      4.3480
_shelx_estimated_absorpt_T_max   0.440
_shelx_estimated_absorpt_T_min   0.167
_exptl_absorpt_coefficient_mu    16.379
_exptl_absorpt_correction_T_max  0.32130
_exptl_absorpt_correction_T_min  0.23454
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -2 3 0.0519
6 2 -3 0.0519
0 -8 -2 0.0818
0 8 2 0.0818
-4 1 -4 0.0288
4 -1 4 0.0288

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.3704 -1.5219 2.7181 0.0849 0.1080 -0.9905
6.3704 1.5219 -2.7181 -0.0849 -0.1080 0.9905
0.2004 -8.4582 -1.5641 -0.5940 -0.7762 -0.2116
-0.2004 8.4582 1.5641 0.5940 0.7762 0.2116
-3.7042 1.1424 -4.4290 0.7606 -0.5819 -0.2878
3.7042 -1.1424 4.4290 -0.7606 0.5819 0.2878

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9690
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.868
_diffrn_reflns_theta_min         4.355
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00 -38.00   0.50    0.50    --  -46.45 101.00 -89.00   74
  2  ω    -35.00  18.00   0.50    0.50    --  -46.45 101.00 -89.00  106
  3  ω     62.00  88.00   0.50    0.50    --  107.75-101.00 166.00   52
  4  ω    112.00 170.00   0.50    0.50    --  107.75 101.00 -89.00  116
  5  ω     -7.00  19.00   0.50    0.50    --  -46.45  19.00-120.00   52
  6  ω    -21.00  17.00   0.50    0.50    --  -46.45  38.00  30.00   76
  7  ω     -3.00  28.00   0.50    0.50    --  -46.45  19.00 -90.00   62
  8  ω     -7.00  25.00   0.50    0.50    --  -46.45  19.00   0.00   64
  9  ω      5.00  56.00   0.50    0.50    --   46.45-101.00 166.00  102
 10  ω     35.00  87.00   0.50    0.50    --  107.75 -61.00-150.00  104
 11  ω     32.00  59.00   0.50    0.50    --  107.75 -30.00-180.00   54
 12  ω     39.00  73.00   0.50    0.50    --  107.75 -45.00 -90.00   68
 13  ω     47.00  73.00   0.50    0.50    --  107.75 -45.00 -30.00   52
 14  ω     36.00  66.00   0.50    0.50    --  107.75 -45.00  60.00   60
 15  ω     55.00  81.00   0.50    0.50    --  107.75 -95.00-150.00   52
 16  ω     46.00  72.00   0.50    0.50    --  107.75-125.00   0.00   52
 17  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00-120.00   50
 18  ω     34.00 121.00   0.50    0.50    --  107.75 -77.00-180.00  174
 19  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00 120.00   50
 20  ω     35.00  85.00   0.50    0.50    --  107.75 -61.00-120.00  100
 21  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00  60.00   50
 22  ω     95.00 163.00   0.50    0.50    --  107.75 125.00 -30.00  136
 23  ω    113.00 139.00   0.50    0.50    --  107.75  45.00 150.00   52
 24  ω    152.00 177.00   0.50    0.50    --  107.75  45.00 150.00   50
 25  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00-150.00   50
 26  ω     94.00 148.00   0.50    0.50    --  107.75 125.00-180.00  108
 27  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 28  ω     74.00  99.00   0.50    0.50    --  107.75 -95.00-120.00   50
 29  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00 150.00   50
 30  ω     40.00  67.00   0.50    0.50    --  107.75 -45.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0719130000
_diffrn_orient_matrix_UB_12      0.0850964000
_diffrn_orient_matrix_UB_13      -0.0896457000
_diffrn_orient_matrix_UB_21      0.0223450000
_diffrn_orient_matrix_UB_22      0.0682038000
_diffrn_orient_matrix_UB_23      0.1302833000
_diffrn_orient_matrix_UB_31      0.1317223000
_diffrn_orient_matrix_UB_32      0.0348274000
_diffrn_orient_matrix_UB_33      -0.0361964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2571
_reflns_number_total             2774
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.774
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2774
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+0.6654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C8(H8), C9(H9), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.72448(2) 0.61069(2) 0.53104(2) 0.03566(11) Uani 1 1 d . . . . .
O5 O 0.5218(4) 0.6083(3) 0.7424(5) 0.0557(10) Uani 1 1 d . . . . .
O2 O 0.4917(4) 0.6322(3) 0.2662(5) 0.0585(10) Uani 1 1 d . . . . .
O1 O 0.7077(5) 0.8420(3) 0.5566(5) 0.0678(11) Uani 1 1 d . . . . .
N1 N 0.7337(3) 0.4497(3) 0.5151(4) 0.0418(9) Uani 1 1 d . . . . .
O4 O 0.9607(5) 0.6193(4) 0.7923(6) 0.0743(14) Uani 1 1 d . . . . .
O3 O 0.9372(5) 0.6347(4) 0.3350(5) 0.0725(12) Uani 1 1 d . . . . .
C2 C 0.5729(5) 0.6200(3) 0.3600(6) 0.0416(10) Uani 1 1 d . . . . .
C7 C 0.7570(4) 0.2600(4) 0.4905(4) 0.0391(8) Uani 1 1 d . . . . .
C4 C 0.8763(6) 0.6122(4) 0.6993(6) 0.0474(12) Uani 1 1 d . . . . .
C5 C 0.5932(5) 0.6054(3) 0.6652(6) 0.0399(10) Uani 1 1 d . . . . .
C6 C 0.7427(5) 0.3637(4) 0.5055(5) 0.0413(9) Uani 1 1 d . . . . .
C12 C 0.6874(5) 0.1939(4) 0.5613(5) 0.0451(10) Uani 1 1 d . . . . .
H12 H 0.629941 0.218775 0.619340 0.054 Uiso 1 1 calc R U . . .
C10 C 0.7874(4) 0.0575(4) 0.4642(4) 0.0452(10) Uani 1 1 d . . . . .
H10 H 0.799377 -0.012197 0.456839 0.054 Uiso 1 1 calc R U . . .
C8 C 0.8407(5) 0.2244(4) 0.4044(5) 0.0437(10) Uani 1 1 d . . . . .
H8 H 0.886839 0.269223 0.355077 0.052 Uiso 1 1 calc R U . . .
C1 C 0.7152(5) 0.7574(4) 0.5464(5) 0.0445(10) Uani 1 1 d . . . . .
C3 C 0.8587(6) 0.6237(4) 0.4014(6) 0.0469(12) Uani 1 1 d . . . . .
C9 C 0.8560(6) 0.1221(4) 0.3916(6) 0.0471(12) Uani 1 1 d . . . . .
H9 H 0.913000 0.096585 0.333532 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7018(6) 0.0934(4) 0.5471(6) 0.0512(12) Uani 1 1 d . . . . .
H11 H 0.653348 0.048623 0.593898 0.061 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
W1 N1 2.175(5) . ?
W1 C2 2.059(5) . ?
W1 C4 2.039(6) . ?
W1 C5 2.045(5) . ?
W1 C1 1.984(5) . ?
W1 C3 2.042(6) . ?
O5 C5 1.143(7) . ?
O2 C2 1.127(7) . ?
O1 C1 1.146(7) . ?
N1 C6 1.166(7) . ?
O4 C4 1.134(8) . ?
O3 C3 1.133(7) . ?
C7 C6 1.414(7) . ?
C7 C12 1.401(7) . ?
C7 C8 1.392(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.370(8) . ?
C10 H10 0.9500 . ?
C10 C9 1.391(7) . ?
C10 C11 1.387(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(7) . ?
C9 H9 0.9500 . ?
C11 H11 0.9500 . ?

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
C2 W1 N1 92.30(16) . . ?
C4 W1 N1 91.67(16) . . ?
C4 W1 C2 175.9(2) . . ?
C4 W1 C5 89.8(2) . . ?
C4 W1 C3 88.8(2) . . ?
C5 W1 N1 93.04(16) . . ?
C5 W1 C2 90.9(2) . . ?
C1 W1 N1 179.61(17) . . ?
C1 W1 C2 87.70(18) . . ?
C1 W1 C4 88.34(19) . . ?
C1 W1 C5 86.57(18) . . ?
C1 W1 C3 90.5(2) . . ?
C3 W1 N1 89.90(19) . . ?
C3 W1 C2 90.3(2) . . ?
C3 W1 C5 176.8(2) . . ?
C6 N1 W1 177.8(3) . . ?
O2 C2 W1 175.0(4) . . ?
C12 C7 C6 120.3(4) . . ?
C8 C7 C6 119.3(4) . . ?
C8 C7 C12 120.4(5) . . ?
O4 C4 W1 175.7(5) . . ?
O5 C5 W1 175.8(4) . . ?
N1 C6 C7 177.9(5) . . ?
C7 C12 H12 119.9 . . ?
C11 C12 C7 120.2(5) . . ?
C11 C12 H12 119.9 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C11 C10 C9 120.8(5) . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 119.1(4) . . ?
C9 C8 H8 120.5 . . ?
O1 C1 W1 178.6(5) . . ?
O3 C3 W1 176.0(6) . . ?
C10 C9 C8 119.7(5) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C12 C11 C10 119.7(5) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 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
C7 C12 C11 C10 1.1(8) . . . . ?
C7 C8 C9 C10 0.2(8) . . . . ?
C6 C7 C12 C11 -179.7(5) . . . . ?
C6 C7 C8 C9 179.1(4) . . . . ?
C12 C7 C8 C9 -1.1(7) . . . . ?
C8 C7 C12 C11 0.4(7) . . . . ?
C9 C10 C11 C12 -2.0(8) . . . . ?
C11 C10 C9 C8 1.3(8) . . . . ?


_ins_header                      
;
TITL RMK_365_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.332470  13.458264   9.665321  90.0000 100.7130  90.0000
ZERR    4.00   0.000148   0.000209   0.000140   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O W
UNIT 48.00 20.00 4.00 20.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.06 0.13 0.17
TREF
HKLF 4
END
;
_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 2.287
_oxdiff_exptl_absorpt_empirical_full_min 0.696
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/hexane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_366_scale
_database_code_depnum_ccdc_archive 'CCDC 2403980'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 N O5 Sb W'
_chemical_formula_sum            'C14 H18 N O5 Sb W'
_chemical_formula_weight         585.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C18H14O5N1Sb1W1 '
_chemical_oxdiff_usercomment     'benzene evap '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   22.5380(2)
_cell_length_b                   14.13850(14)
_cell_length_c                   6.04179(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1925.24(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6993
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.7850
_cell_measurement_theta_min      3.1080
_shelx_estimated_absorpt_T_max   0.220
_shelx_estimated_absorpt_T_min   0.032
_exptl_absorpt_coefficient_mu    22.182
_exptl_absorpt_correction_T_max  0.14258
_exptl_absorpt_correction_T_min  0.04345
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent dark colourless'
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -9 0 0.0656
-3 9 0 0.0656
-3 -1 4 0.1408
3 1 -4 0.2784
15 0 0 0.0490
-15 0 0 0.0490

_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.098
_exptl_crystal_size_rad          0.111
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.9216 -8.9911 -0.0479 -0.2324 -0.9719 0.0382
-2.9216 8.9911 0.0479 0.2324 0.9719 -0.0382
-2.8710 -1.1915 3.8122 -0.0106 -0.0366 0.9993
2.9752 0.8909 -3.8215 0.0027 0.0039 -1.0000
14.5531 0.1313 -0.4001 0.8611 -0.4091 -0.3019
-14.5531 -0.1313 0.4001 -0.8611 0.4091 0.3019

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            8281
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.039
_diffrn_reflns_theta_min         3.923
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  28.00   0.50    0.50    --  -46.45  17.00 -96.00   52
  2  ω     72.00 110.00   0.50    0.50    --   46.45-149.00-137.00   76
  3  ω     95.00 172.00   0.50    0.50    --  107.75 123.00 105.00  154
  4  ω     42.00  90.00   0.50    0.50    --  107.75-111.00 -72.00   96
  5  ω    108.00 178.00   0.50    0.50    --  107.75  17.00 -96.00  140
  6  ω     -8.00  29.00   0.50    0.50    --  -46.45  19.00-180.00   74
  7  ω     -6.00  21.00   0.50    0.50    --  -46.45  19.00  30.00   54
  8  ω     -5.00  23.00   0.50    0.50    --  -46.45  19.00 -30.00   56
  9  ω     -8.00  23.00   0.50    0.50    --  -46.45  19.00 120.00   62
 10  ω     39.00  69.00   0.50    0.50    --  107.75 -45.00-120.00   60
 11  ω     35.00  60.00   0.50    0.50    --  107.75 -45.00  90.00   50
 12  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 150.00   50
 13  ω     78.00 112.00   0.50    0.50    --  107.75-125.00   0.00   68
 14  ω     43.00  69.00   0.50    0.50    --  107.75-125.00   0.00   52
 15  ω     83.00 108.00   0.50    0.50    --  107.75-125.00 -30.00   50
 16  ω     35.00  69.00   0.50    0.50    --  107.75 -45.00 -30.00   68
 17  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00  90.00   50
 18  ω     38.00  73.00   0.50    0.50    --  107.75 -45.00  60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0603227000
_diffrn_orient_matrix_UB_12      0.0451521000
_diffrn_orient_matrix_UB_13      0.0567707000
_diffrn_orient_matrix_UB_21      -0.0290191000
_diffrn_orient_matrix_UB_22      0.0986656000
_diffrn_orient_matrix_UB_23      -0.0006209000
_diffrn_orient_matrix_UB_31      -0.0138192000
_diffrn_orient_matrix_UB_32      -0.0100576000
_diffrn_orient_matrix_UB_33      0.2485713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2063
_reflns_number_total             2113
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0743P)²+0.8736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1003
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.80898(2) 0.250000 0.54704(5) 0.04252(14) Uani 1 2 d S T P . .
Sb1 Sb 0.60708(2) 0.250000 0.08275(6) 0.03387(14) Uani 1 2 d S T P . .
N1 N 0.6839(2) 0.250000 0.2677(12) 0.0491(13) Uani 1 2 d S T P . .
O2 O 0.85796(18) 0.0958(3) 0.2104(7) 0.0646(9) Uani 1 1 d . . . . .
O3 O 0.75272(19) 0.4104(4) 0.8545(8) 0.0781(12) Uani 1 1 d . . . . .
C4 C 0.7282(3) 0.250000 0.3644(12) 0.0438(12) Uani 1 2 d S T P . .
C2 C 0.84045(19) 0.1499(3) 0.3330(8) 0.0475(9) Uani 1 1 d . . . . .
C3 C 0.7734(2) 0.3533(4) 0.7459(9) 0.0558(11) Uani 1 1 d . . . . .
C5 C 0.5710(2) 0.3748(3) 0.2501(7) 0.0411(8) Uani 1 1 d . . . . .
O1 O 0.9294(2) 0.250000 0.8175(11) 0.0762(17) Uani 1 2 d S T P . .
C1 C 0.8850(3) 0.250000 0.7184(13) 0.0537(16) Uani 1 2 d S T P . .
C6 C 0.5065(2) 0.3822(4) 0.1756(13) 0.0688(15) Uani 1 1 d . . . . .
H6A H 0.504690 0.382096 0.013537 0.103 Uiso 1 1 calc R U . . .
H6B H 0.489217 0.441036 0.232181 0.103 Uiso 1 1 calc R U . . .
H6C H 0.484040 0.328148 0.233283 0.103 Uiso 1 1 calc R U . . .
C7 C 0.5747(4) 0.3728(4) 0.5010(9) 0.0681(16) Uani 1 1 d . . . . .
H7A H 0.546962 0.325543 0.558784 0.102 Uiso 1 1 calc R U . . .
H7B H 0.564407 0.435263 0.559924 0.102 Uiso 1 1 calc R U . . .
H7C H 0.615197 0.356383 0.546142 0.102 Uiso 1 1 calc R U . . .
C8 C 0.6071(3) 0.4570(4) 0.1595(11) 0.0609(13) Uani 1 1 d . . . . .
H8A H 0.648899 0.448539 0.198962 0.091 Uiso 1 1 calc R U . . .
H8B H 0.592394 0.516310 0.223020 0.091 Uiso 1 1 calc R U . . .
H8C H 0.603109 0.459074 -0.001974 0.091 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
W1 C4 2.128(6) . ?
W1 C2 2.044(5) . ?
W1 C2 2.044(5) 7_565 ?
W1 C3 2.054(5) . ?
W1 C3 2.054(5) 7_565 ?
W1 C1 2.001(7) . ?
Sb1 N1 2.061(5) . ?
Sb1 C5 2.190(4) 7_565 ?
Sb1 C5 2.190(4) . ?
N1 C4 1.157(9) . ?
O2 C2 1.135(6) . ?
O3 C3 1.140(7) . ?
C5 C6 1.527(7) . ?
C5 C7 1.518(7) . ?
C5 C8 1.520(6) . ?
O1 C1 1.168(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
C2 W1 C4 88.21(18) 7_565 . ?
C2 W1 C4 88.21(18) . . ?
C2 W1 C2 87.6(3) . 7_565 ?
C2 W1 C3 90.8(2) 7_565 . ?
C2 W1 C3 176.17(18) 7_565 7_565 ?
C2 W1 C3 90.8(2) . 7_565 ?
C2 W1 C3 176.17(18) . . ?
C3 W1 C4 88.27(18) 7_565 . ?
C3 W1 C4 88.27(18) . . ?
C3 W1 C3 90.7(3) . 7_565 ?
C1 W1 C4 179.9(3) . . ?
C1 W1 C2 91.7(2) . . ?
C1 W1 C2 91.7(2) . 7_565 ?
C1 W1 C3 91.8(2) . 7_565 ?
C1 W1 C3 91.8(2) . . ?
N1 Sb1 C5 93.52(16) . 7_565 ?
N1 Sb1 C5 93.52(16) . . ?
C5 Sb1 C5 107.4(2) 7_565 . ?
C4 N1 Sb1 177.5(6) . . ?
N1 C4 W1 179.1(6) . . ?
O2 C2 W1 178.5(4) . . ?
O3 C3 W1 178.7(4) . . ?
C6 C5 Sb1 105.8(3) . . ?
C7 C5 Sb1 115.2(3) . . ?
C7 C5 C6 110.3(5) . . ?
C7 C5 C8 110.1(5) . . ?
C8 C5 Sb1 104.6(3) . . ?
C8 C5 C6 110.5(4) . . ?
O1 C1 W1 179.7(7) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?


_ins_header                      
;
TITL RMK_366_scale in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 1.54184  22.538038  14.138502   6.041789  90.0000  90.0000  90.0000
ZERR    4.00   0.000202   0.000141   0.000050   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O Sb W
UNIT 72.00 56.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.10 0.15 0.49
TREF
HKLF 4
END
;
_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 2.186
_oxdiff_exptl_absorpt_empirical_full_min 0.674
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: benzene'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_361_a_scale
_database_code_depnum_ccdc_archive 'CCDC 2403973'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-09-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 Cr N O5 P'
_chemical_formula_sum            'C14 H18 Cr N O5 P'
_chemical_formula_weight         363.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H18N1P1O5Cr1
_chemical_oxdiff_usercomment     'benzene evap'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   21.7679(3)
_cell_length_b                   13.5735(2)
_cell_length_c                   5.92480(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1750.58(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6700
_cell_measurement_theta_min      3.8220
_shelx_estimated_absorpt_T_max   0.512
_shelx_estimated_absorpt_T_min   0.126
_exptl_absorpt_coefficient_mu    6.431
_exptl_absorpt_correction_T_max  0.35752
_exptl_absorpt_correction_T_min  0.27915
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 4 1 0.1682
-14 0 1 0.1921
3 -4 -1 0.0749
14 -1 -1 0.2909
-1 0 -9 0.0590
1 0 9 0.0590
-7 3 1 0.1500

_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.139
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.7467 3.6942 0.7501 -0.6195 0.0172 -0.7848
-14.0485 0.3038 0.6354 0.8841 -0.0214 -0.4668
2.6791 -3.7505 -1.0206 0.2068 -0.0071 0.9784
13.8312 -0.7194 -0.7280 -0.8277 0.0198 0.5608
-0.5931 0.2102 -8.7886 0.0253 0.9980 0.0574
0.5931 -0.2102 8.7886 -0.0253 -0.9980 -0.0574
-6.7324 3.3465 1.1190 0.0983 -0.0044 -0.9952

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7056
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.884
_diffrn_reflns_theta_min         4.062
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  10.00   0.50    0.50    --  -46.45  32.00-117.00   50
  2  ω     30.00  56.00   0.50    0.50    --   46.45-119.00-132.00   52
  3  ω    103.00 129.00   0.50    0.50    --  107.75  92.00  58.00   52
  4  ω    152.00 178.00   0.50    0.50    --  107.75  92.00  58.00   52
  5  ω     35.00  61.00   0.50    0.50    --  107.75 -32.00  83.00   52
  6  ω     73.00 154.00   0.50    0.50    --  107.75 156.00 107.00  162
  7  ω   -102.00 -52.00   0.50    0.50    --  -46.45 -32.00  83.00  100
  8  ω    -21.00  26.00   0.50    0.50    --  -46.45  38.00   0.00   94
  9  ω    -12.00  24.00   0.50    0.50    --  -46.45  38.00  30.00   72
 10  ω     32.00  58.00   0.50    0.50    --  107.75 -30.00  60.00   52
 11  ω     32.00  59.00   0.50    0.50    --  107.75 -30.00  30.00   54
 12  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 150.00   50
 13  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -30.00   50
 14  ω     59.00 122.00   0.50    0.50    --  107.75 -77.00-150.00  126
 15  ω     52.00  92.00   0.50    0.50    --  107.75 -61.00-150.00   80
 16  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00  90.00   50
 17  ω     42.00  70.00   0.50    0.50    --  107.75 -45.00 120.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651665000
_diffrn_orient_matrix_UB_12      -0.1014308000
_diffrn_orient_matrix_UB_13      -0.0009113000
_diffrn_orient_matrix_UB_21      -0.0029111000
_diffrn_orient_matrix_UB_22      0.0304750000
_diffrn_orient_matrix_UB_23      -0.1126339000
_diffrn_orient_matrix_UB_31      0.0274580000
_diffrn_orient_matrix_UB_32      -0.2374236000
_diffrn_orient_matrix_UB_33      -0.0140688000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1847
_reflns_number_total             1919
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1919
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.101
_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)+(0.0732P)²+0.1698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1100
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cr1 Cr 0.19926(2) 0.250000 0.52926(6) 0.02504(16) Uani 1 2 d S T P . .
P1 P 0.39480(2) 0.250000 0.13237(8) 0.01953(17) Uani 1 2 d S T P . .
O2 O 0.14891(6) 0.09614(10) 0.2041(2) 0.0422(3) Uani 1 1 d . . . . .
O1 O 0.08155(8) 0.250000 0.8014(3) 0.0475(5) Uani 1 2 d S T P . .
N1 N 0.32539(9) 0.250000 0.2729(3) 0.0269(4) Uani 1 2 d S T P . .
O3 O 0.25324(7) 0.41034(12) 0.8302(3) 0.0527(4) Uani 1 1 d . . . . .
C4 C 0.27787(10) 0.250000 0.3634(4) 0.0264(5) Uani 1 2 d S T P . .
C5 C 0.42735(7) 0.36474(11) 0.2609(3) 0.0250(3) Uani 1 1 d . . . . .
C1 C 0.12566(11) 0.250000 0.6981(4) 0.0316(5) Uani 1 2 d S T P . .
C2 C 0.16806(7) 0.15239(13) 0.3287(3) 0.0306(4) Uani 1 1 d . . . . .
C3 C 0.23268(8) 0.35045(14) 0.7191(3) 0.0354(4) Uani 1 1 d . . . . .
C7 C 0.38806(9) 0.44786(13) 0.1630(3) 0.0390(4) Uani 1 1 d . . . . .
H7A H 0.386339 0.441461 -0.001669 0.059 Uiso 1 1 calc R U . . .
H7B H 0.406260 0.511569 0.202793 0.059 Uiso 1 1 calc R U . . .
H7C H 0.346405 0.443802 0.225053 0.059 Uiso 1 1 calc R U . . .
C8 C 0.49320(9) 0.37569(15) 0.1695(4) 0.0429(4) Uani 1 1 d . . . . .
H8A H 0.520440 0.329811 0.248853 0.064 Uiso 1 1 calc R U . . .
H8B H 0.507450 0.443351 0.193900 0.064 Uiso 1 1 calc R U . . .
H8C H 0.493636 0.360894 0.007629 0.064 Uiso 1 1 calc R U . . .
C6 C 0.42699(12) 0.37192(15) 0.5173(3) 0.0425(5) Uani 1 1 d . . . . .
H6A H 0.385970 0.355565 0.574213 0.064 Uiso 1 1 calc R U . . .
H6B H 0.437721 0.439161 0.562887 0.064 Uiso 1 1 calc R U . . .
H6C H 0.457067 0.325659 0.579921 0.064 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
Cr1 C4 1.973(2) . ?
Cr1 C1 1.889(2) . ?
Cr1 C2 1.9051(18) . ?
Cr1 C2 1.9051(18) 7_565 ?
Cr1 C3 1.9113(19) 7_565 ?
Cr1 C3 1.9113(19) . ?
P1 N1 1.7251(19) . ?
P1 C5 1.8728(16) . ?
P1 C5 1.8728(16) 7_565 ?
O2 C2 1.141(2) . ?
O1 C1 1.139(3) . ?
N1 C4 1.165(3) . ?
O3 C3 1.138(2) . ?
C5 C7 1.530(2) . ?
C5 C8 1.540(2) . ?
C5 C6 1.522(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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 Cr1 C4 177.90(10) . . ?
C1 Cr1 C2 91.60(7) . . ?
C1 Cr1 C2 91.60(7) . 7_565 ?
C1 Cr1 C3 90.64(7) . 7_565 ?
C1 Cr1 C3 90.64(7) . . ?
C2 Cr1 C4 89.91(7) 7_565 . ?
C2 Cr1 C4 89.91(7) . . ?
C2 Cr1 C2 88.13(10) . 7_565 ?
C2 Cr1 C3 90.39(8) 7_565 . ?
C2 Cr1 C3 177.34(7) 7_565 7_565 ?
C2 Cr1 C3 90.39(8) . 7_565 ?
C2 Cr1 C3 177.34(7) . . ?
C3 Cr1 C4 87.89(7) . . ?
C3 Cr1 C4 87.89(7) 7_565 . ?
C3 Cr1 C3 91.02(12) . 7_565 ?
N1 P1 C5 97.76(6) . 7_565 ?
N1 P1 C5 97.76(6) . . ?
C5 P1 C5 112.53(10) . 7_565 ?
C4 N1 P1 178.5(2) . . ?
N1 C4 Cr1 177.5(2) . . ?
C7 C5 P1 104.34(11) . . ?
C7 C5 C8 108.42(15) . . ?
C8 C5 P1 106.84(11) . . ?
C6 C5 P1 117.20(12) . . ?
C6 C5 C7 109.17(15) . . ?
C6 C5 C8 110.45(17) . . ?
O1 C1 Cr1 179.5(2) . . ?
O2 C2 Cr1 177.94(16) . . ?
O3 C3 Cr1 179.07(17) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
N1 P1 C5 C7 -69.26(12) . . . . ?
N1 P1 C5 C8 176.02(12) . . . . ?
N1 P1 C5 C6 51.56(16) . . . . ?
C5 P1 C5 C7 -171.04(8) 7_565 . . . ?
C5 P1 C5 C8 74.25(15) 7_565 . . . ?
C5 P1 C5 C6 -50.22(19) 7_565 . . . ?


_ins_header                      
;
TITL RMK_361_A_scale in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  21.767924   5.924773  13.573534  90.0000  90.0000  90.0000
ZERR    4.00   0.000313   0.000087   0.000215   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y+1/2, z 
SYMM -x+1/2, y+1/2, z+1/2 
SFAC C H N O P Cr
UNIT 56.00 72.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.12 0.24 0.55
TREF
HKLF 4
END
;
_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 2.037
_oxdiff_exptl_absorpt_empirical_full_min 0.575
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: benzene'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_363_a_scale
_database_code_depnum_ccdc_archive 'CCDC 2403976'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-09-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 Mo N O5 P'
_chemical_formula_sum            'C14 H18 Mo N O5 P'
_chemical_formula_weight         407.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H18N1O5P1Mo1
_chemical_oxdiff_usercomment     'benzene evap'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   22.1456(2)
_cell_length_b                   13.6345(2)
_cell_length_c                   5.93730(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1792.73(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7205
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.7930
_cell_measurement_theta_min      3.2430
_shelx_estimated_absorpt_T_max   0.382
_shelx_estimated_absorpt_T_min   0.144
_exptl_absorpt_coefficient_mu    7.016
_exptl_absorpt_correction_T_max  0.27732
_exptl_absorpt_correction_T_min  0.18279
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       sphere
_exptl_crystal_F_000             824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 -1 0 0.1341
0 0 9 0.1976
-14 1 0 0.1626
0 0 -9 0.2446
1 4 0 0.0716
0 -4 0 0.0946

_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.17
_exptl_crystal_size_rad          0.174
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
14.2297 -0.5463 -0.0023 -0.0230 -0.0335 -0.9992
-0.4866 0.0400 8.8449 0.5217 0.8531 -0.0054
-14.2297 0.5462 -0.0229 0.0215 0.0311 0.9993
-0.1928 -0.0139 -8.8496 -0.5209 -0.8520 0.0531
0.5994 3.8506 -0.0854 -0.8485 0.5192 0.1022
-0.3469 -3.8528 0.0912 0.8469 -0.5182 -0.1197

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7801
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.010
_diffrn_reflns_theta_min         3.992
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  19.00   0.50    0.50    --  -46.45  11.00-110.00   56
  2  ω    -75.00 -49.00   0.50    0.50    --  -46.45 129.00  94.00   52
  3  ω     97.00 123.00   0.50    0.50    --  107.75 129.00  94.00   52
  4  ω     90.00 167.00   0.50    0.50    --  107.75  11.00-110.00  154
  5  ω    132.00 170.00   0.50    0.50    --  107.75 118.00  11.00   76
  6  ω     -8.00  29.00   0.50    0.50    --  -46.45  19.00 -90.00   74
  7  ω     -7.00  18.00   0.50    0.50    --  -46.45  19.00 -60.00   50
  8  ω     -2.00  24.00   0.50    0.50    --  -46.45  19.00-150.00   52
  9  ω     -1.00  25.00   0.50    0.50    --  -46.45  19.00-180.00   52
 10  ω     41.00  86.00   0.50    0.50    --   46.45-118.00 -75.00   90
 11  ω     36.00 105.00   0.50    0.50    --  107.75 -95.00 -60.00  138
 12  ω     71.00  98.00   0.50    0.50    --  107.75 -95.00  30.00   54
 13  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00  90.00   50
 14  ω     38.00  63.00   0.50    0.50    --  107.75 -95.00  30.00   50
 15  ω     41.00  73.00   0.50    0.50    --  107.75 -45.00 -90.00   64
 16  ω     44.00  72.00   0.50    0.50    --  107.75 -95.00   0.00   56
 17  ω     80.00 105.00   0.50    0.50    --  107.75 -95.00   0.00   50
 18  ω     35.00  72.00   0.50    0.50    --  107.75 -45.00-120.00   74
 19  ω     35.00  60.00   0.50    0.50    --  107.75 -45.00   0.00   50
 20  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099566000
_diffrn_orient_matrix_UB_12      -0.2174981000
_diffrn_orient_matrix_UB_13      0.0594181000
_diffrn_orient_matrix_UB_21      0.0029028000
_diffrn_orient_matrix_UB_22      0.1365016000
_diffrn_orient_matrix_UB_23      0.0959953000
_diffrn_orient_matrix_UB_31      -0.0687920000
_diffrn_orient_matrix_UB_32      0.0371511000
_diffrn_orient_matrix_UB_33      -0.0045633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1954
_reflns_number_total             1971
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.433
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.111
_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)+(0.0581P)²+1.0174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0904
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.80099(2) 0.250000 0.52780(4) 0.02534(13) Uani 1 2 d S T P . .
P1 P 0.60202(3) 0.250000 0.12554(11) 0.02091(17) Uani 1 2 d S T P . .
O2 O 0.85369(8) 0.09036(13) 0.1889(3) 0.0435(4) Uani 1 1 d . . . . .
O1 O 0.92149(11) 0.250000 0.8133(5) 0.0477(7) Uani 1 2 d S T P . .
N1 N 0.67087(11) 0.250000 0.2624(4) 0.0265(5) Uani 1 2 d S T P . .
O3 O 0.74579(9) 0.41820(16) 0.8400(4) 0.0548(5) Uani 1 1 d . . . . .
C4 C 0.71761(14) 0.250000 0.3491(6) 0.0278(6) Uani 1 2 d S T P . .
C5 C 0.57060(10) 0.36445(15) 0.2545(4) 0.0259(4) Uani 1 1 d . . . . .
C1 C 0.87845(14) 0.250000 0.7099(6) 0.0332(7) Uani 1 2 d S T P . .
C2 C 0.83458(10) 0.14593(17) 0.3122(4) 0.0305(5) Uani 1 1 d . . . . .
C7 C 0.60938(11) 0.44733(17) 0.1569(5) 0.0379(5) Uani 1 1 d . . . . .
H7A H 0.650680 0.441771 0.214791 0.057 Uiso 1 1 calc R U . . .
H7B H 0.592336 0.510778 0.201316 0.057 Uiso 1 1 calc R U . . .
H7C H 0.609907 0.442409 -0.007743 0.057 Uiso 1 1 calc R U . . .
C3 C 0.76547(11) 0.35806(19) 0.7313(4) 0.0358(5) Uani 1 1 d . . . . .
C6 C 0.57157(16) 0.3713(2) 0.5106(4) 0.0422(7) Uani 1 1 d . . . . .
H6A H 0.541768 0.325888 0.573760 0.063 Uiso 1 1 calc R U . . .
H6B H 0.561689 0.438470 0.556730 0.063 Uiso 1 1 calc R U . . .
H6C H 0.611880 0.354125 0.566069 0.063 Uiso 1 1 calc R U . . .
C8 C 0.50579(10) 0.37536(18) 0.1671(5) 0.0414(6) Uani 1 1 d . . . . .
H8A H 0.504827 0.361383 0.005206 0.062 Uiso 1 1 calc R U . . .
H8B H 0.491720 0.442510 0.193763 0.062 Uiso 1 1 calc R U . . .
H8C H 0.479390 0.329150 0.246391 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
Mo1 C4 2.130(3) . ?
Mo1 C1 2.028(3) . ?
Mo1 C2 2.051(2) 7_565 ?
Mo1 C2 2.051(2) . ?
Mo1 C3 2.061(2) 7_565 ?
Mo1 C3 2.061(2) . ?
P1 N1 1.728(3) . ?
P1 C5 1.872(2) 7_565 ?
P1 C5 1.872(2) . ?
O2 C2 1.136(3) . ?
O1 C1 1.134(4) . ?
N1 C4 1.156(4) . ?
O3 C3 1.131(3) . ?
C5 C7 1.533(3) . ?
C5 C6 1.524(3) . ?
C5 C8 1.534(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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 Mo1 C4 177.65(13) . . ?
C1 Mo1 C2 91.49(9) . 7_565 ?
C1 Mo1 C2 91.49(9) . . ?
C1 Mo1 C3 90.58(9) . . ?
C1 Mo1 C3 90.58(9) . 7_565 ?
C2 Mo1 C4 90.21(9) . . ?
C2 Mo1 C4 90.21(9) 7_565 . ?
C2 Mo1 C2 87.58(13) . 7_565 ?
C2 Mo1 C3 90.56(10) . 7_565 ?
C2 Mo1 C3 90.56(10) 7_565 . ?
C2 Mo1 C3 177.25(9) 7_565 7_565 ?
C2 Mo1 C3 177.25(9) . . ?
C3 Mo1 C4 87.77(9) . . ?
C3 Mo1 C4 87.78(9) 7_565 . ?
C3 Mo1 C3 91.24(15) . 7_565 ?
N1 P1 C5 97.79(9) . 7_565 ?
N1 P1 C5 97.79(9) . . ?
C5 P1 C5 112.91(13) 7_565 . ?
C4 N1 P1 178.4(3) . . ?
N1 C4 Mo1 176.6(3) . . ?
C7 C5 P1 104.58(15) . . ?
C7 C5 C8 108.96(19) . . ?
C6 C5 P1 117.02(17) . . ?
C6 C5 C7 108.9(2) . . ?
C6 C5 C8 110.2(2) . . ?
C8 C5 P1 106.87(15) . . ?
O1 C1 Mo1 179.5(3) . . ?
O2 C2 Mo1 178.1(2) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C3 Mo1 178.9(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
N1 P1 C5 C7 68.55(17) . . . . ?
N1 P1 C5 C6 -52.0(2) . . . . ?
N1 P1 C5 C8 -176.00(17) . . . . ?
C5 P1 C5 C7 170.46(11) 7_565 . . . ?
C5 P1 C5 C6 49.9(3) 7_565 . . . ?
C5 P1 C5 C8 -74.1(2) 7_565 . . . ?


_ins_header                      
;
TITL RMK_363_A_scale in Pna2(1) 
REM Pna2(1) (#33, found as Pc2(1)n in cab setting)
CELL 1.54184  22.145605   5.937315  13.634531  90.0000  90.0000  90.0000
ZERR    4.00   0.000245   0.000077   0.000166   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y+1/2, z 
SYMM -x+1/2, y+1/2, z+1/2 
SFAC C H N O P Mo
UNIT 56.00 72.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.17 0.32 0.45
TREF
HKLF 4
END
;
_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 2.650
_oxdiff_exptl_absorpt_empirical_full_min 0.602
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: benzene'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_360_scale
_database_code_depnum_ccdc_archive 'CCDC 2403977'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-09-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 As N O5 W'
_chemical_formula_sum            'C14 H18 As N O5 W'
_chemical_formula_weight         539.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H18As1W1N1O5
_chemical_oxdiff_usercomment     'benzene evap'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   22.2713(2)
_cell_length_b                   13.80740(10)
_cell_length_c                   5.94700(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1828.75(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6068
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6180
_cell_measurement_theta_min      3.1200
_shelx_estimated_absorpt_T_max   0.543
_shelx_estimated_absorpt_T_min   0.091
_exptl_absorpt_coefficient_mu    13.901
_exptl_absorpt_correction_T_max  0.34913
_exptl_absorpt_correction_T_min  0.26864
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -3 3 0.0696
2 9 0 0.1009
3 -3 -4 0.0736
14 0 0 0.0238
-14 -1 0 0.0099

_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.066
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9982 -3.4167 3.4028 -0.0399 -0.0611 -0.9973
2.0735 8.8604 -0.1882 0.4802 0.7836 0.3943
2.6967 -3.2354 -3.5273 -0.3322 -0.5464 0.7688
14.4415 -0.2845 -0.0895 -0.8164 0.5000 0.2889
-14.4253 -0.5269 -0.0731 0.7628 -0.5835 -0.2788

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.051
_diffrn_reflns_theta_min         3.970
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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  -6.00   0.50    0.50    --  -46.45 103.00  17.00   52
  2  ω    106.00 150.00   0.50    0.50    --  107.75 100.00 -76.00   88
  3  ω     33.00  58.00   0.50    0.50    --  107.75 -33.00  15.00   50
  4  ω     96.00 145.00   0.50    0.50    --  107.75  33.00 174.00   98
  5  ω    149.00 176.00   0.50    0.50    --  107.75  33.00 174.00   54
  6  ω     36.00  75.00   0.50    0.50    --  107.75-103.00 -84.00   78
  7  ω     -5.00  20.00   0.50    0.50    --  -46.45  19.00-150.00   50
  8  ω     -8.00  28.00   0.50    0.50    --  -46.45  19.00 -30.00   72
  9  ω     -9.00  21.00   0.50    0.50    --  -46.45  33.00 174.00   60
 10  ω     -8.00  28.00   0.50    0.50    --  -46.45  19.00 -90.00   72
 11  ω    -22.00  13.00   0.50    0.50    --  -46.45  38.00 120.00   70
 12  ω     32.00  58.00   0.50    0.50    --  107.75 -30.00 150.00   52
 13  ω     40.00  68.00   0.50    0.50    --  107.75 -45.00 -90.00   56
 14  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00   0.00   50
 15  ω     63.00 109.00   0.50    0.50    --  107.75-125.00 -90.00   92
 16  ω     36.00  66.00   0.50    0.50    --  107.75 -45.00 150.00   60
 17  ω     38.00  73.00   0.50    0.50    --  107.75 -61.00   0.00   70
 18  ω     52.00  89.00   0.50    0.50    --  107.75 -61.00-120.00   74
 19  ω     38.00  70.00   0.50    0.50    --  107.75 -45.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0552730000
_diffrn_orient_matrix_UB_12      0.0669274000
_diffrn_orient_matrix_UB_13      -0.0094628000
_diffrn_orient_matrix_UB_21      0.0369060000
_diffrn_orient_matrix_UB_22      0.0820897000
_diffrn_orient_matrix_UB_23      0.1078358000
_diffrn_orient_matrix_UB_31      0.0192387000
_diffrn_orient_matrix_UB_32      0.0349952000
_diffrn_orient_matrix_UB_33      -0.2353476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1955
_reflns_number_total             2010
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.699
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.188
_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     112
_refine_ls_number_reflns         2010
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0485P)²+7.8339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0944
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.80419(2) 0.750000 0.46688(6) 0.02800(13) Uani 1 2 d S T P . .
As1 As 0.60282(3) 0.750000 0.89493(12) 0.02270(18) Uani 1 2 d S T P . .
O2 O 0.85557(19) 0.9079(3) 0.8059(7) 0.0459(10) Uani 1 1 d . . . . .
N1 N 0.6768(3) 0.750000 0.7401(11) 0.0335(13) Uani 1 2 d S T P . .
O1 O 0.9255(3) 0.750000 0.1858(12) 0.0546(17) Uani 1 2 d S T P . .
C5 C 0.5708(2) 0.6303(3) 0.7469(8) 0.0291(10) Uani 1 1 d . . . . .
C2 C 0.8371(2) 0.8532(4) 0.6820(9) 0.0330(11) Uani 1 1 d . . . . .
O3 O 0.7479(2) 0.5845(4) 0.1559(9) 0.0593(12) Uani 1 1 d . . . . .
C1 C 0.8803(3) 0.750000 0.2852(14) 0.0358(16) Uani 1 2 d S T P . .
C4 C 0.7217(3) 0.750000 0.6498(13) 0.0292(14) Uani 1 2 d S T P . .
C7 C 0.5732(3) 0.6280(5) 0.4931(10) 0.0471(15) Uani 1 1 d . . . . .
H7A H 0.543357 0.673155 0.432178 0.071 Uiso 1 1 calc R U . . .
H7B H 0.564332 0.562352 0.440193 0.071 Uiso 1 1 calc R U . . .
H7C H 0.613326 0.647133 0.442417 0.071 Uiso 1 1 calc R U . . .
C8 C 0.5063(2) 0.6210(4) 0.8283(13) 0.0466(14) Uani 1 1 d . . . . .
H8A H 0.504757 0.632278 0.990887 0.070 Uiso 1 1 calc R U . . .
H8B H 0.491353 0.555842 0.794925 0.070 Uiso 1 1 calc R U . . .
H8C H 0.481204 0.669043 0.751412 0.070 Uiso 1 1 calc R U . . .
C3 C 0.7680(2) 0.6444(5) 0.2657(10) 0.0396(12) Uani 1 1 d . . . . .
C6 C 0.6087(3) 0.5491(4) 0.8415(11) 0.0409(12) Uani 1 1 d . . . . .
H6A H 0.649906 0.555081 0.785292 0.061 Uiso 1 1 calc R U . . .
H6B H 0.591934 0.486715 0.794553 0.061 Uiso 1 1 calc R U . . .
H6C H 0.608840 0.552982 1.006060 0.061 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
W1 C2 2.051(6) . ?
W1 C2 2.051(6) 7_575 ?
W1 C1 2.011(7) . ?
W1 C4 2.134(7) . ?
W1 C3 2.051(6) . ?
W1 C3 2.051(6) 7_575 ?
As1 N1 1.888(6) . ?
As1 C5 2.003(5) . ?
As1 C5 2.003(5) 7_575 ?
O2 C2 1.132(7) . ?
N1 C4 1.135(10) . ?
O1 C1 1.166(9) . ?
C5 C7 1.510(7) . ?
C5 C8 1.522(7) . ?
C5 C6 1.511(7) . ?
O3 C3 1.145(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
C2 W1 C2 88.1(3) 7_575 . ?
C2 W1 C4 89.41(19) . . ?
C2 W1 C4 89.40(19) 7_575 . ?
C2 W1 C3 176.8(2) . . ?
C2 W1 C3 176.8(2) 7_575 7_575 ?
C2 W1 C3 90.6(2) 7_575 . ?
C1 W1 C2 91.9(2) . . ?
C1 W1 C2 91.9(2) . 7_575 ?
C1 W1 C4 178.1(3) . . ?
C1 W1 C3 91.0(2) . 7_575 ?
C1 W1 C3 91.0(2) . . ?
C3 W1 C2 90.6(2) 7_575 . ?
C3 W1 C4 87.7(2) . . ?
C3 W1 C4 87.7(2) 7_575 . ?
C3 W1 C3 90.6(3) 7_575 . ?
N1 As1 C5 95.51(19) . . ?
N1 As1 C5 95.51(19) . 7_575 ?
C5 As1 C5 111.2(3) 7_575 . ?
C4 N1 As1 179.1(7) . . ?
C7 C5 As1 116.4(4) . . ?
C7 C5 C8 110.4(5) . . ?
C7 C5 C6 109.7(5) . . ?
C8 C5 As1 105.4(4) . . ?
C6 C5 As1 104.5(3) . . ?
C6 C5 C8 110.3(5) . . ?
O2 C2 W1 177.7(5) . . ?
O1 C1 W1 177.9(7) . . ?
N1 C4 W1 177.6(7) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C3 W1 179.0(6) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?


_ins_header                      
;
TITL RMK_360_scale in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 1.54184  22.271304  13.807379   5.946994  90.0000  90.0000  90.0000
ZERR    4.00   0.000215   0.000130   0.000062   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O As W
UNIT 56.00 72.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.05 0.23 0.33
TREF
HKLF 4
END
;
_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 2.703
_oxdiff_exptl_absorpt_empirical_full_min 0.669
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: benzene'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_381_b_2_scale2
_database_code_depnum_ccdc_archive 'CCDC 2403972'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2025-02-13 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H23 N O2 P Re'
_chemical_formula_sum            'C16 H23 N O2 P Re'
_chemical_formula_weight         478.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H23N1O2P1Re1
_chemical_oxdiff_usercomment     'hexane at -30 deg '
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5007(4)
_cell_length_b                   10.3978(6)
_cell_length_c                   12.9967(6)
_cell_angle_alpha                91.653(4)
_cell_angle_beta                 94.080(4)
_cell_angle_gamma                93.172(5)
_cell_volume                     874.44(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4211
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      3.8340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.043
_exptl_absorpt_correction_T_max  0.367
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             464
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 18 0.1086
-9 2 3 0.1079
-1 -1 -18 0.0748
9 -2 -5 0.1768
0 15 0 0.1108
-1 -15 2 0.0706

_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.195
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.2068 1.6178 18.1165 -0.2830 0.1732 -0.9433
-9.0683 2.1194 3.3091 0.7548 -0.4626 -0.4651
-0.8543 -1.3859 -17.9141 0.3744 -0.2292 0.8985
8.8629 -2.2657 -5.4673 -0.7006 0.4294 0.5700
0.1686 14.6027 0.2472 0.5153 0.8408 -0.1658
-0.5000 -14.5551 1.5157 -0.5213 -0.8508 0.0657

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.273
_diffrn_reflns_theta_min         3.414
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  37.00   1.00    1.00    --   -9.26  77.00  30.00   74
  2  ω    -34.00  16.00   1.00    1.00    --   -9.26 -77.00 -90.00   50
  3  ω    -37.00  42.00   1.00    1.00    --    9.42 -77.00 150.00   79
  4  ω    -19.00  82.00   1.00    1.00    --    9.42  57.00 -60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0819236000
_diffrn_orient_matrix_UB_12      0.0365683000
_diffrn_orient_matrix_UB_13      -0.0198238000
_diffrn_orient_matrix_UB_21      0.0661856000
_diffrn_orient_matrix_UB_22      0.0567277000
_diffrn_orient_matrix_UB_23      0.0052500000
_diffrn_orient_matrix_UB_31      0.0302279000
_diffrn_orient_matrix_UB_32      -0.0108409000
_diffrn_orient_matrix_UB_33      -0.0507576000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3340
_reflns_number_total             3780
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.349
_refine_diff_density_min         -2.131
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.040
_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)+(0.0280P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0824
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(O2)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C16(H16), C15(H15), C14(H14)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C),
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Re1 Re 0.52370(3) 0.40046(2) 0.80658(2) 0.01604(10) Uani 1 1 d . . . . .
P1 P 0.1639(3) 0.76850(18) 0.71730(13) 0.0230(4) Uani 1 1 d . . . . .
O2 O 0.2611(7) 0.2785(5) 0.9668(3) 0.0264(9) Uani 1 1 d . . . . .
O1 O 0.2452(7) 0.2768(5) 0.6271(3) 0.0335(12) Uani 1 1 d . . . . .
N1 N 0.2993(8) 0.6564(5) 0.7846(4) 0.0210(12) Uani 1 1 d . . . . .
C3 C 0.3752(9) 0.5570(6) 0.7947(4) 0.0187(14) Uani 1 1 d . . . . .
C2 C 0.3507(10) 0.3272(7) 0.9050(5) 0.0264(9) Uani 1 1 d . . . . .
C12 C 0.8247(9) 0.3271(7) 0.7526(5) 0.0249(16) Uani 1 1 d . . . . .
H12 H 0.823955 0.267530 0.697763 0.030 Uiso 1 1 calc R U . . .
C1 C 0.3471(9) 0.3231(7) 0.6961(5) 0.0205(14) Uani 1 1 d . . . . .
C13 C 0.8138(9) 0.2973(7) 0.8569(5) 0.0245(16) Uani 1 1 d . . . . .
H13 H 0.805221 0.215103 0.883258 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8371(9) 0.4632(7) 0.7446(5) 0.0247(16) Uani 1 1 d . . . . .
H16 H 0.846154 0.508670 0.684397 0.030 Uiso 1 1 calc R U . . .
C15 C 0.8332(9) 0.5161(8) 0.8455(5) 0.0285(17) Uani 1 1 d . . . . .
H15 H 0.839352 0.603494 0.863553 0.034 Uiso 1 1 calc R U . . .
C14 C 0.8184(9) 0.4146(7) 0.9143(5) 0.0235(16) Uani 1 1 d . . . . .
H14 H 0.812559 0.423396 0.985408 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2286(10) 0.9131(7) 0.8032(5) 0.0246(15) Uani 1 1 d . . . . .
C4 C 0.3151(12) 0.7719(8) 0.5983(5) 0.0348(19) Uani 1 1 d . . . . .
C10 C 0.4499(11) 0.9676(9) 0.8153(6) 0.047(2) Uani 1 1 d . . . . .
H10A H 0.539083 0.900759 0.835529 0.070 Uiso 1 1 calc R U . . .
H10B H 0.462716 1.035672 0.867300 0.070 Uiso 1 1 calc R U . . .
H10C H 0.488455 1.001025 0.750901 0.070 Uiso 1 1 calc R U . . .
C7 C 0.2479(15) 0.6439(8) 0.5410(6) 0.052(2) Uani 1 1 d . . . . .
H7A H 0.289269 0.573654 0.582634 0.078 Uiso 1 1 calc R U . . .
H7B H 0.311936 0.639698 0.476795 0.078 Uiso 1 1 calc R U . . .
H7C H 0.100445 0.638088 0.527797 0.078 Uiso 1 1 calc R U . . .
C9 C 0.0893(12) 1.0192(8) 0.7643(7) 0.048(2) Uani 1 1 d . . . . .
H9A H 0.125263 1.043611 0.696940 0.071 Uiso 1 1 calc R U . . .
H9B H 0.108183 1.092777 0.811012 0.071 Uiso 1 1 calc R U . . .
H9C H -0.052570 0.987230 0.760761 0.071 Uiso 1 1 calc R U . . .
C6 C 0.5513(11) 0.7803(10) 0.6185(5) 0.049(2) Uani 1 1 d . . . . .
H6A H 0.596066 0.863864 0.647732 0.073 Uiso 1 1 calc R U . . .
H6B H 0.613991 0.766739 0.554714 0.073 Uiso 1 1 calc R U . . .
H6C H 0.591491 0.715348 0.665809 0.073 Uiso 1 1 calc R U . . .
C5 C 0.2447(14) 0.8836(8) 0.5325(6) 0.049(2) Uani 1 1 d . . . . .
H5A H 0.096575 0.879141 0.523286 0.073 Uiso 1 1 calc R U . . .
H5B H 0.301228 0.877621 0.466437 0.073 Uiso 1 1 calc R U . . .
H5C H 0.292091 0.964016 0.566691 0.073 Uiso 1 1 calc R U . . .
C11 C 0.1635(16) 0.8763(9) 0.9100(6) 0.063(3) Uani 1 1 d . . . . .
H11A H 0.027625 0.834499 0.903200 0.095 Uiso 1 1 calc R U . . .
H11B H 0.162757 0.952657 0.953266 0.095 Uiso 1 1 calc R U . . .
H11C H 0.259404 0.818833 0.940302 0.095 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
Re1 C3 1.943(7) . ?
Re1 C2 1.910(6) . ?
Re1 C12 2.288(6) . ?
Re1 C1 1.903(7) . ?
Re1 C13 2.286(6) . ?
Re1 C16 2.311(6) . ?
Re1 C15 2.303(7) . ?
Re1 C14 2.286(6) . ?
P1 N1 1.721(5) . ?
P1 C8 1.857(7) . ?
P1 C4 1.890(7) . ?
O2 C2 1.139(7) . ?
O1 C1 1.154(7) . ?
N1 C3 1.176(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.405(9) . ?
C12 C16 1.420(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.409(10) . ?
C16 H16 0.9300 . ?
C16 C15 1.410(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.406(10) . ?
C14 H14 0.9300 . ?
C8 C10 1.513(9) . ?
C8 C9 1.539(10) . ?
C8 C11 1.532(9) . ?
C4 C7 1.533(11) . ?
C4 C6 1.537(10) . ?
C4 C5 1.533(10) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

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
C3 Re1 C12 136.8(3) . . ?
C3 Re1 C13 150.5(3) . . ?
C3 Re1 C16 101.9(3) . . ?
C3 Re1 C15 91.8(3) . . ?
C3 Re1 C14 115.9(3) . . ?
C2 Re1 C3 94.3(3) . . ?
C2 Re1 C12 128.2(3) . . ?
C2 Re1 C13 96.8(3) . . ?
C2 Re1 C16 154.5(3) . . ?
C2 Re1 C15 125.4(3) . . ?
C2 Re1 C14 95.6(3) . . ?
C12 Re1 C16 36.0(2) . . ?
C12 Re1 C15 59.3(3) . . ?
C1 Re1 C3 89.5(3) . . ?
C1 Re1 C2 90.7(3) . . ?
C1 Re1 C12 96.5(3) . . ?
C1 Re1 C13 117.5(3) . . ?
C1 Re1 C16 108.9(2) . . ?
C1 Re1 C15 143.6(2) . . ?
C1 Re1 C14 153.2(3) . . ?
C13 Re1 C12 35.8(2) . . ?
C13 Re1 C16 59.9(2) . . ?
C13 Re1 C15 59.6(3) . . ?
C13 Re1 C14 35.9(2) . . ?
C15 Re1 C16 35.6(2) . . ?
C14 Re1 C12 59.5(2) . . ?
C14 Re1 C16 59.6(2) . . ?
C14 Re1 C15 35.7(2) . . ?
N1 P1 C8 99.9(3) . . ?
N1 P1 C4 98.6(3) . . ?
C8 P1 C4 111.9(3) . . ?
C3 N1 P1 154.5(5) . . ?
N1 C3 Re1 174.7(6) . . ?
O2 C2 Re1 174.5(6) . . ?
Re1 C12 H12 121.1 . . ?
C13 C12 Re1 72.0(4) . . ?
C13 C12 H12 125.6 . . ?
C13 C12 C16 108.8(6) . . ?
C16 C12 Re1 72.9(4) . . ?
C16 C12 H12 125.6 . . ?
O1 C1 Re1 177.8(5) . . ?
Re1 C13 H13 121.3 . . ?
C12 C13 Re1 72.2(4) . . ?
C12 C13 H13 126.2 . . ?
C12 C13 C14 107.5(6) . . ?
C14 C13 Re1 72.1(4) . . ?
C14 C13 H13 126.2 . . ?
Re1 C16 H16 122.2 . . ?
C12 C16 Re1 71.1(3) . . ?
C12 C16 H16 126.6 . . ?
C15 C16 Re1 71.9(4) . . ?
C15 C16 C12 106.9(6) . . ?
C15 C16 H16 126.6 . . ?
Re1 C15 H15 121.9 . . ?
C16 C15 Re1 72.5(4) . . ?
C16 C15 H15 125.7 . . ?
C14 C15 Re1 71.5(4) . . ?
C14 C15 C16 108.6(7) . . ?
C14 C15 H15 125.7 . . ?
Re1 C14 H14 121.0 . . ?
C13 C14 Re1 72.0(4) . . ?
C13 C14 H14 125.9 . . ?
C15 C14 Re1 72.8(3) . . ?
C15 C14 C13 108.3(6) . . ?
C15 C14 H14 125.9 . . ?
C10 C8 P1 118.9(5) . . ?
C10 C8 C9 108.9(6) . . ?
C10 C8 C11 108.1(7) . . ?
C9 C8 P1 107.0(5) . . ?
C11 C8 P1 106.0(5) . . ?
C11 C8 C9 107.5(6) . . ?
C7 C4 P1 103.8(5) . . ?
C7 C4 C6 108.9(7) . . ?
C6 C4 P1 115.5(5) . . ?
C5 C4 P1 108.4(5) . . ?
C5 C4 C7 109.2(6) . . ?
C5 C4 C6 110.6(7) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
Re1 C12 C13 C14 -63.8(4) . . . . ?
Re1 C12 C16 C15 63.4(4) . . . . ?
Re1 C13 C14 C15 -64.3(4) . . . . ?
Re1 C16 C15 C14 62.9(4) . . . . ?
Re1 C15 C14 C13 63.8(4) . . . . ?
N1 P1 C8 C10 65.9(6) . . . . ?
N1 P1 C8 C9 -170.4(5) . . . . ?
N1 P1 C8 C11 -55.9(6) . . . . ?
N1 P1 C4 C7 73.2(5) . . . . ?
N1 P1 C4 C6 -46.0(7) . . . . ?
N1 P1 C4 C5 -170.7(5) . . . . ?
C12 C13 C14 Re1 63.9(4) . . . . ?
C12 C13 C14 C15 -0.3(7) . . . . ?
C12 C16 C15 Re1 -62.9(4) . . . . ?
C12 C16 C15 C14 -0.1(7) . . . . ?
C13 C12 C16 Re1 -63.6(4) . . . . ?
C13 C12 C16 C15 -0.1(7) . . . . ?
C16 C12 C13 Re1 64.1(4) . . . . ?
C16 C12 C13 C14 0.3(7) . . . . ?
C16 C15 C14 Re1 -63.5(4) . . . . ?
C16 C15 C14 C13 0.3(7) . . . . ?
C8 P1 N1 C3 -164.8(12) . . . . ?
C8 P1 C4 C7 177.6(5) . . . . ?
C8 P1 C4 C6 58.4(7) . . . . ?
C8 P1 C4 C5 -66.3(6) . . . . ?
C4 P1 N1 C3 -50.7(13) . . . . ?
C4 P1 C8 C10 -37.6(6) . . . . ?
C4 P1 C8 C9 86.1(5) . . . . ?
C4 P1 C8 C11 -159.4(5) . . . . ?


_ins_header                      
;
TITL RMK_381_B_2_scale2 in P1 
REM P1 (#1 in standard setting)
CELL 0.71073   6.500669  10.397827  12.996701  91.6526  94.0802  93.1718
ZERR    2.00   0.000358   0.000600   0.000634   0.0043   0.0042   0.0046
LATT -1
SFAC C H N O P Re
UNIT 32.00 46.00 2.00 4.00 2.00 2.00
TREF
HKLF 4
END
;
_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 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.762
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2/hexane'
####################################################################### 
# 
# 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_rmk_325_scale
_database_code_depnum_ccdc_archive 'CCDC 2403970'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-05-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H32 Li2 N6 O10 W2'
_chemical_formula_sum            'C24 H32 Li2 N6 O10 W2'
_chemical_formula_weight         946.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32Li2N6O10W2
_chemical_oxdiff_usercomment     'THF evap at -30 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.71120(10)
_cell_length_b                   10.7852(2)
_cell_length_c                   11.3689(2)
_cell_angle_alpha                112.5180(10)
_cell_angle_beta                 111.564(2)
_cell_angle_gamma                93.9840(10)
_cell_volume                     889.73(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    10165
_cell_measurement_temperature    149(4)
_cell_measurement_theta_max      77.7900
_cell_measurement_theta_min      4.5540
_shelx_estimated_absorpt_T_max   0.346
_shelx_estimated_absorpt_T_min   0.079
_exptl_absorpt_coefficient_mu    12.236
_exptl_absorpt_correction_T_max  0.27716
_exptl_absorpt_correction_T_min  0.18262
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 6 0.0980
0 -6 -1 0.1112
1 7 -3 0.1901
-5 1 1 0.0428
1 -1 -6 0.0124
2 1 5 0.0777
4 1 1 0.0803

_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.100
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.6969 0.4155 6.2875 0.7926 -0.6070 0.0574
-0.2194 -5.6642 -1.0093 -0.4475 0.3449 -0.8251
0.7585 6.8484 -3.0784 0.0154 -0.0146 0.9998
-5.4856 0.9322 0.9935 -0.6857 -0.7239 -0.0754
0.6736 -0.6085 -6.1837 -0.7910 0.6058 -0.0856
1.7066 0.7953 4.5894 0.9534 -0.2272 0.1985
4.4828 0.6744 1.0285 0.8876 0.3695 0.2750

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.051
_diffrn_reflns_theta_min         4.577
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  58.00   0.50    0.50    --   46.45 -34.00  54.00   84
  2  ω    -28.00   9.00   0.50    0.50    --   46.45 -34.00  54.00   74
  3  ω     33.00 120.00   0.50    0.50    --   46.45  34.00-147.00  174
  4  ω     32.00  61.00   0.50    0.50    --  107.75 -34.00  54.00   58
  5  ω    142.00 168.00   0.50    0.50    --  107.75  34.00-147.00   52
  6  ω     95.00 133.00   0.50    0.50    --  107.75  34.00-147.00   76
  7  ω     -6.00  21.00   0.50    0.50    --  -46.45  34.00-147.00   54
  8  ω    -58.00 -33.00   0.50    0.50    --  -46.45 -38.00 150.00   50
  9  ω    -86.00 -18.00   0.50    0.50    --  -46.45 125.00 -90.00  136
 10  ω   -121.00 -33.00   0.50    0.50    --  -46.45 -34.00  54.00  176
 11  ω   -120.00 -68.00   0.50    0.50    --  -46.45 -38.00 150.00  104
 12  ω     59.00  86.00   0.50    0.50    --   46.45-125.00 -60.00   54
 13  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00-150.00   50
 14  ω     81.00 106.00   0.50    0.50    --  107.75 -95.00-180.00   50
 15  ω     99.00 128.00   0.50    0.50    --  107.75 125.00  90.00   58
 16  ω     44.00  70.00   0.50    0.50    --  107.75 -45.00-180.00   52
 17  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 18  ω     67.00 111.00   0.50    0.50    --  107.75-125.00 150.00   88
 19  ω     51.00  87.00   0.50    0.50    --  107.75 -61.00-120.00   72
 20  ω     64.00 105.00   0.50    0.50    --  107.75 -95.00 -90.00   82
 21  ω     32.00  59.00   0.50    0.50    --  107.75 -30.00-120.00   54
 22  ω     36.00  76.00   0.50    0.50    --  107.75 -95.00-180.00   80
 23  ω     87.00 117.00   0.50    0.50    --  107.75 -77.00-180.00   60
 24  ω     34.00  79.00   0.50    0.50    --  107.75 -77.00-180.00   90
 25  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -30.00   50
 26  ω     36.00  70.00   0.50    0.50    --  107.75 -95.00 -30.00   68
 27  ω     78.00 104.00   0.50    0.50    --  107.75 -95.00 -30.00   52
 28  ω     39.00  73.00   0.50    0.50    --  107.75 -45.00  30.00   68
 29  ω    102.00 139.00   0.50    0.50    --  107.75  30.00 -90.00   74
 30  ω    146.00 171.00   0.50    0.50    --  107.75  30.00 -90.00   50
 31  ω     95.00 138.00   0.50    0.50    --  107.75 125.00 150.00   86
 32  ω    145.00 171.00   0.50    0.50    --  107.75 125.00 150.00   52
 33  ω     39.00  70.00   0.50    0.50    --  107.75 -61.00 120.00   62
 34  ω     52.00 103.00   0.50    0.50    --  107.75 -95.00  60.00  102
 35  ω     78.00 104.00   0.50    0.50    --  107.75 -95.00  30.00   52
 36  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -90.00   50
 37  ω     45.00  71.00   0.50    0.50    --  107.75-100.00 163.50   52
 38  ω     94.00 175.00   0.50    0.50    --  107.75  30.00 150.00  162
 39  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00  60.00   50
 40  ω     32.00  58.00   0.50    0.50    --  107.75 -30.00   0.00   52
 41  ω     79.00 107.00   0.50    0.50    --  107.75-100.00 163.50   56
 42  ω     36.00  65.00   0.50    0.50    --  107.75 -95.00  30.00   58
 43  ω     97.00 140.00   0.50    0.50    --  107.75  45.00 -30.00   86
 44  ω    145.00 176.00   0.50    0.50    --  107.75  45.00 -30.00   62
 45  ω     69.00  95.00   0.50    0.50    --  107.75 -95.00  90.00   52
 46  ω     44.00 106.00   0.50    0.50    --  107.75 -95.00-120.00  124
 47  ω     41.00  66.00   0.50    0.50    --  107.75-125.00 -60.00   50
 48  ω    138.00 173.00   0.50    0.50    --  107.75 125.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1585761000
_diffrn_orient_matrix_UB_12      0.0478289000
_diffrn_orient_matrix_UB_13      0.1404839000
_diffrn_orient_matrix_UB_21      0.1086665000
_diffrn_orient_matrix_UB_22      -0.0506438000
_diffrn_orient_matrix_UB_23      -0.0811456000
_diffrn_orient_matrix_UB_31      0.0388459000
_diffrn_orient_matrix_UB_32      0.1434600000
_diffrn_orient_matrix_UB_33      0.0039522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3677
_reflns_number_total             3729
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.214
_refine_diff_density_min         -2.720
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.056
_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)+(0.0570P)²+2.5208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0945
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C11 \\sim N3-C11'
 with sigma of 0.02
 N3-C12 \\sim N3-C12'
 with sigma of 0.02
 N3-C10 \\sim N3-C10'
 with sigma of 0.02
 C9-C10 \\sim C9-C10'
 with sigma of 0.02
3. Others
 Sof(H9bc)=Sof(H9bd)=Sof(C10')=Sof(H10c)=Sof(H10d)=Sof(C11')=Sof(H11d)=
 Sof(H11e)=Sof(H11f)=Sof(C12')=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(H9aa)=Sof(H9ab)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=Sof(C12)=Sof(H12a)=
 Sof(H12b)=Sof(H12c)=Sof(C10)=Sof(H10a)=Sof(H10b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9aa,H9ab), C9(H9bc,H9bd), C10(H10a,H10b), C10'(H10c,H10d)
4.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C8(H8a,H8b,H8c),
 C11'(H11d,H11e,H11f), C12'(H12d,H12e,H12f)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.71211(3) 0.78660(2) 0.32347(2) 0.03180(10) Uani 1 1 d . . . . .
O5 O 0.6950(6) 0.5240(5) 0.0618(5) 0.0493(10) Uani 1 1 d . . . . .
O4 O 1.0749(6) 0.7553(6) 0.4961(5) 0.0589(12) Uani 1 1 d . . . . .
O2 O 0.3316(6) 0.7789(5) 0.1371(5) 0.0615(12) Uani 1 1 d . . . . .
O3 O 0.7255(8) 1.0536(5) 0.5825(5) 0.0632(13) Uani 1 1 d . . . . .
O1 O 0.8764(8) 0.9817(5) 0.2303(5) 0.0658(14) Uani 1 1 d . . . . .
N1 N 0.5632(7) 0.5882(5) 0.4401(5) 0.0454(11) Uani 1 1 d . . . . .
N3 N 0.4171(7) 0.2334(5) 0.2255(5) 0.0466(11) Uani 1 1 d D . . . .
C5 C 0.6994(6) 0.6164(5) 0.1557(5) 0.0348(10) Uani 1 1 d . . . . .
C6 C 0.6126(7) 0.6577(5) 0.3978(5) 0.0368(10) Uani 1 1 d . . . . .
N2 N 0.1485(6) 0.3741(7) 0.2230(6) 0.0569(13) Uani 1 1 d . . . . .
C1 C 0.8138(8) 0.9100(6) 0.2639(6) 0.0437(12) Uani 1 1 d . . . . .
C4 C 0.9468(7) 0.7714(6) 0.4371(6) 0.0424(12) Uani 1 1 d . . . . .
C2 C 0.4654(8) 0.7829(6) 0.2039(6) 0.0412(11) Uani 1 1 d . . . . .
C3 C 0.7222(8) 0.9585(6) 0.4921(6) 0.0417(12) Uani 1 1 d . . . . .
C9 C 0.1343(10) 0.2519(10) 0.0965(9) 0.077(2) Uani 1 1 d D . . . .
H9AA H 0.015751 0.201491 0.040107 0.092 Uiso 0.762(19) 1 calc R U P A 1
H9AB H 0.171150 0.283737 0.039915 0.092 Uiso 0.762(19) 1 calc R U P A 1
H9BC H 0.062933 0.172186 0.086888 0.092 Uiso 0.238(19) 1 calc R U P A 2
H9BD H 0.074764 0.267482 0.014617 0.092 Uiso 0.238(19) 1 calc R U P A 2
C7 C 0.1253(11) 0.4906(11) 0.1870(10) 0.078(2) Uani 1 1 d . . . . .
H7A H 0.212876 0.512154 0.160652 0.116 Uiso 1 1 calc R U . . .
H7B H 0.131980 0.569918 0.267024 0.116 Uiso 1 1 calc R U . . .
H7C H 0.015893 0.465906 0.109634 0.116 Uiso 1 1 calc R U . . .
C11 C 0.4982(17) 0.1414(11) 0.2825(13) 0.065(3) Uani 0.762(19) 1 d D . P A 1
H11A H 0.494907 0.059018 0.206912 0.098 Uiso 0.762(19) 1 calc R U P A 1
H11B H 0.438391 0.117000 0.329572 0.098 Uiso 0.762(19) 1 calc R U P A 1
H11C H 0.614462 0.188009 0.348202 0.098 Uiso 0.762(19) 1 calc R U P A 1
C12 C 0.5021(15) 0.2605(12) 0.1461(12) 0.062(3) Uani 0.762(19) 1 d D . P A 1
H12A H 0.620339 0.304252 0.207315 0.093 Uiso 0.762(19) 1 calc R U P A 1
H12B H 0.450393 0.320379 0.107776 0.093 Uiso 0.762(19) 1 calc R U P A 1
H12C H 0.491828 0.174778 0.070797 0.093 Uiso 0.762(19) 1 calc R U P A 1
C8 C 0.0247(11) 0.3500(13) 0.2733(12) 0.092(3) Uani 1 1 d . . . . .
H8A H -0.087938 0.329342 0.201245 0.138 Uiso 1 1 calc R U . . .
H8B H 0.041358 0.431356 0.355741 0.138 Uiso 1 1 calc R U . . .
H8C H 0.038255 0.273412 0.296264 0.138 Uiso 1 1 calc R U . . .
Li1 Li 0.3952(11) 0.4083(9) 0.3695(9) 0.0366(17) Uani 1 1 d . . . . .
C10 C 0.2348(11) 0.1586(9) 0.1314(9) 0.057(3) Uani 0.762(19) 1 d D . P A 1
H10A H 0.226711 0.084499 0.045544 0.068 Uiso 0.762(19) 1 calc R U P A 1
H10B H 0.189561 0.117584 0.178054 0.068 Uiso 0.762(19) 1 calc R U P A 1
C10' C 0.286(3) 0.217(4) 0.092(2) 0.071(10) Uiso 0.238(19) 1 d D . P A 2
H10C H 0.332925 0.273592 0.058824 0.085 Uiso 0.238(19) 1 calc R U P A 2
H10D H 0.257376 0.121116 0.023342 0.085 Uiso 0.238(19) 1 calc R U P A 2
C11' C 0.421(7) 0.117(4) 0.261(6) 0.085(15) Uiso 0.238(19) 1 d D . P A 2
H11D H 0.489912 0.062169 0.224974 0.128 Uiso 0.238(19) 1 calc R U P A 2
H11E H 0.307301 0.061284 0.219370 0.128 Uiso 0.238(19) 1 calc R U P A 2
H11F H 0.468238 0.151028 0.361259 0.128 Uiso 0.238(19) 1 calc R U P A 2
C12' C 0.577(4) 0.274(4) 0.215(4) 0.065(9) Uiso 0.238(19) 1 d D . P A 2
H12D H 0.673142 0.290587 0.300480 0.097 Uiso 0.238(19) 1 calc R U P A 2
H12E H 0.578052 0.356479 0.201864 0.097 Uiso 0.238(19) 1 calc R U P A 2
H12F H 0.582770 0.200500 0.136836 0.097 Uiso 0.238(19) 1 calc R U P A 2


_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
W1 C5 2.038(5) . ?
W1 C6 2.161(5) . ?
W1 C1 1.995(6) . ?
W1 C4 2.035(6) . ?
W1 C2 2.066(6) . ?
W1 C3 2.062(5) . ?
O5 C5 1.133(7) . ?
O4 C4 1.136(8) . ?
O2 C2 1.121(8) . ?
O3 C3 1.130(7) . ?
O1 C1 1.167(7) . ?
N1 C6 1.166(7) . ?
N1 Li1 2.025(9) . ?
N1 Li1 2.044(10) 2_666 ?
N3 C11 1.469(9) . ?
N3 C12 1.453(10) . ?
N3 Li1 2.046(10) . ?
N3 C10 1.493(10) . ?
N3 C10' 1.460(19) . ?
N3 C11' 1.46(2) . ?
N3 C12' 1.489(19) . ?
N2 C9 1.488(11) . ?
N2 C7 1.468(10) . ?
N2 C8 1.445(9) . ?
N2 Li1 2.078(10) . ?
C9 H9AA 0.9700 . ?
C9 H9AB 0.9700 . ?
C9 H9BC 0.9700 . ?
C9 H9BD 0.9700 . ?
C9 C10 1.452(12) . ?
C9 C10' 1.41(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
Li1 Li1 2.660(17) 2_666 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C11' H11F 0.9600 . ?
C12' H12D 0.9600 . ?
C12' H12E 0.9600 . ?
C12' H12F 0.9600 . ?

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
C5 W1 C6 91.0(2) . . ?
C5 W1 C2 88.9(2) . . ?
C5 W1 C3 179.4(2) . . ?
C1 W1 C5 90.5(2) . . ?
C1 W1 C6 177.2(2) . . ?
C1 W1 C4 91.0(3) . . ?
C1 W1 C2 93.4(2) . . ?
C1 W1 C3 89.6(2) . . ?
C4 W1 C5 88.0(2) . . ?
C4 W1 C6 86.7(2) . . ?
C4 W1 C2 174.6(2) . . ?
C4 W1 C3 92.6(2) . . ?
C2 W1 C6 88.9(2) . . ?
C3 W1 C6 88.8(2) . . ?
C3 W1 C2 90.5(2) . . ?
C6 N1 Li1 140.5(5) . . ?
C6 N1 Li1 137.9(5) . 2_666 ?
Li1 N1 Li1 81.6(4) . 2_666 ?
C11 N3 Li1 115.1(6) . . ?
C11 N3 C10 106.8(7) . . ?
C12 N3 C11 108.3(8) . . ?
C12 N3 Li1 113.8(6) . . ?
C12 N3 C10 110.7(7) . . ?
C10 N3 Li1 101.6(5) . . ?
C10' N3 Li1 102.9(12) . . ?
C10' N3 C12' 102.5(19) . . ?
C11' N3 Li1 114(2) . . ?
C11' N3 C10' 119(3) . . ?
C11' N3 C12' 110(3) . . ?
C12' N3 Li1 106.1(15) . . ?
O5 C5 W1 178.2(5) . . ?
N1 C6 W1 178.2(5) . . ?
C9 N2 Li1 102.9(5) . . ?
C7 N2 C9 108.4(7) . . ?
C7 N2 Li1 111.8(6) . . ?
C8 N2 C9 113.2(8) . . ?
C8 N2 C7 108.9(7) . . ?
C8 N2 Li1 111.5(6) . . ?
O1 C1 W1 178.6(6) . . ?
O4 C4 W1 176.3(5) . . ?
O2 C2 W1 178.7(5) . . ?
O3 C3 W1 178.5(6) . . ?
N2 C9 H9AA 109.0 . . ?
N2 C9 H9AB 109.0 . . ?
N2 C9 H9BC 107.8 . . ?
N2 C9 H9BD 107.8 . . ?
H9AA C9 H9AB 107.8 . . ?
H9BC C9 H9BD 107.1 . . ?
C10 C9 N2 113.0(7) . . ?
C10 C9 H9AA 109.0 . . ?
C10 C9 H9AB 109.0 . . ?
C10' C9 N2 118.0(14) . . ?
C10' C9 H9BC 107.8 . . ?
C10' C9 H9BD 107.8 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 Li1 N1 98.4(4) . 2_666 ?
N1 Li1 N3 116.2(4) 2_666 . ?
N1 Li1 N3 117.4(5) . . ?
N1 Li1 N2 120.0(5) 2_666 . ?
N1 Li1 N2 118.2(5) . . ?
N1 Li1 Li1 49.5(3) . 2_666 ?
N1 Li1 Li1 48.9(3) 2_666 2_666 ?
N3 Li1 N2 88.3(4) . . ?
N3 Li1 Li1 133.6(6) . 2_666 ?
N2 Li1 Li1 138.1(6) . 2_666 ?
N3 C10 H10A 109.4 . . ?
N3 C10 H10B 109.4 . . ?
C9 C10 N3 111.0(7) . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N3 C10' H10C 108.4 . . ?
N3 C10' H10D 108.4 . . ?
C9 C10' N3 115.5(16) . . ?
C9 C10' H10C 108.4 . . ?
C9 C10' H10D 108.4 . . ?
H10C C10' H10D 107.5 . . ?
N3 C11' H11D 109.5 . . ?
N3 C11' H11E 109.5 . . ?
N3 C11' H11F 109.5 . . ?
H11D C11' H11E 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
N3 C12' H12D 109.5 . . ?
N3 C12' H12E 109.5 . . ?
N3 C12' H12F 109.5 . . ?
H12D C12' H12E 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?

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
N2 C9 C10 N3 -55.3(10) . . . . ?
N2 C9 C10' N3 39(3) . . . . ?
C7 N2 C9 C10 150.4(8) . . . . ?
C7 N2 C9 C10' 102.4(18) . . . . ?
C11 N3 C10 C9 166.3(8) . . . . ?
C12 N3 C10 C9 -75.9(9) . . . . ?
C8 N2 C9 C10 -88.7(9) . . . . ?
C8 N2 C9 C10' -136.6(17) . . . . ?
Li1 N3 C10 C9 45.3(9) . . . . ?
Li1 N3 C10' C9 -37(3) . . . . ?
Li1 N2 C9 C10 31.8(9) . . . . ?
Li1 N2 C9 C10' -16.1(18) . . . . ?
C11' N3 C10' C9 91(4) . . . . ?
C12' N3 C10' C9 -147(3) . . . . ?


_ins_header                      
;
TITL RMK_325_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.711187  10.785237  11.368916 112.5179 111.5643  93.9840
ZERR    1.00   0.000149   0.000160   0.000179   0.0014   0.0015   0.0013
LATT  1
SFAC C H Li N O W
UNIT 24.00 32.00 2.00 6.00 10.00 2.00
REM  CrysAlisPro recorded range (K): Min=146.2; max=150.0; aver:148.1
TEMP -125
SIZE 0.11 0.19 0.42
TREF
HKLF 4
END
;
_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 5.489
_oxdiff_exptl_absorpt_empirical_full_min 0.484
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_rmk_365_a_scale
_database_code_depnum_ccdc_archive 'CCDC 2403978'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-06-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H11 N O5 W'
_chemical_formula_sum            'C15 H11 N O5 W'
_chemical_formula_weight         469.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H11N1O5W1
_chemical_oxdiff_usercomment     'Et2O/hexane at 0 deg'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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                   9.21210(10)
_cell_length_b                   15.24780(10)
_cell_length_c                   11.81920(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.5200(10)
_cell_angle_gamma                90
_cell_volume                     1614.17(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10261
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.8870
_cell_measurement_theta_min      2.8860
_shelx_estimated_absorpt_T_max   0.346
_shelx_estimated_absorpt_T_min   0.140
_exptl_absorpt_coefficient_mu    13.468
_exptl_absorpt_correction_T_max  0.27269
_exptl_absorpt_correction_T_min  0.17688
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent dark colourless'
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 3 -3 0.0751
2 -9 3 0.0996
-6 -3 3 0.1196
-5 4 1 0.0870
0 6 6 0.0496
0 -5 -6 0.0438
0 9 -4 0.1175

_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.098
_exptl_crystal_size_rad          0.092
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.5337 3.0153 -3.3343 -0.2799 -0.4606 -0.8423
1.6860 -8.5535 2.6093 -0.4111 -0.6702 0.6179
-5.5567 -2.9285 3.3101 0.2845 0.4680 0.8367
-5.3966 4.0447 0.5782 0.5133 0.8399 0.1765
0.1930 5.6042 6.0832 0.8996 -0.4279 -0.0868
-0.0870 -5.4002 -6.2219 -0.9016 0.4289 0.0562
0.2110 8.5197 -3.8526 0.2343 0.4967 -0.8357

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.142
_diffrn_reflns_theta_min         4.819
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  26.00   0.50    0.50    --  -46.45  60.00  88.00  110
  2  ω   -115.00 -39.00   0.50    0.50    --  -46.45 -60.00 -51.00  152
  3  ω     50.00  75.00   0.50    0.50    --   46.45  60.00  88.00   50
  4  ω     24.00  62.00   0.50    0.50    --   46.45 -60.00 -51.00   76
  5  ω    102.00 176.00   0.50    0.50    --  107.75  60.00  88.00  148
  6  ω     44.00  75.00   0.50    0.50    --  107.75 -60.00 -51.00   62
  7  ω     -8.00  22.00   0.50    0.50    --  -46.45  19.00  90.00   60
  8  ω      3.00  30.00   0.50    0.50    --  -46.45  19.00-120.00   54
  9  ω     -8.00  29.00   0.50    0.50    --  -46.45  19.00-150.00   74
 10  ω    -22.00   5.00   0.50    0.50    --  -46.45  38.00-120.00   54
 11  ω     37.00  72.00   0.50    0.50    --  107.75 -45.00-180.00   70
 12  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 -60.00   50
 13  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00 150.00   50
 14  ω     35.00  60.00   0.50    0.50    --  107.75 -77.00-120.00   50
 15  ω     32.00  59.00   0.50    0.50    --  107.75 -30.00 -30.00   54
 16  ω     32.00  57.00   0.50    0.50    --  107.75 -30.00  30.00   50
 17  ω     32.00  58.00   0.50    0.50    --  107.75 -30.00-180.00   52
 18  ω     41.00  66.00   0.50    0.50    --  107.75 -45.00   0.00   50
 19  ω     39.00  67.00   0.50    0.50    --  107.75 -45.00 150.00   56
 20  ω     37.00  86.00   0.50    0.50    --  107.75 -95.00 -60.00   98
 21  ω     40.00  77.00   0.50    0.50    --  107.75 -61.00   0.00   74
 22  ω    142.00 167.00   0.50    0.50    --  107.75  45.00-180.00   50
 23  ω     61.00  87.00   0.50    0.50    --  107.75 -61.00  60.00   52
 24  ω     94.00 119.00   0.50    0.50    --  107.75  45.00-180.00   50
 25  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00   0.00   50
 26  ω     88.00 119.00   0.50    0.50    --  107.75 -77.00-120.00   62
 27  ω     34.00  59.00   0.50    0.50    --  107.75 -30.00 -90.00   50
 28  ω     60.00  85.00   0.50    0.50    --  107.75 -61.00-180.00   50
 29  ω     97.00 133.00   0.50    0.50    --  107.75  77.00   0.00   72
 30  ω     41.00  66.00   0.50    0.50    --  107.75 -45.00  90.00   50
 31  ω     46.00  73.00   0.50    0.50    --  107.75 -45.00-120.00   54
 32  ω     37.00  62.00   0.50    0.50    --  107.75 -45.00  30.00   50
 33  ω     44.00  71.00   0.50    0.50    --  107.75 -61.00  90.00   54
 34  ω     33.00  58.00   0.50    0.50    --  107.75 -30.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0351524000
_diffrn_orient_matrix_UB_12      0.0675944000
_diffrn_orient_matrix_UB_13      0.0867329000
_diffrn_orient_matrix_UB_21      -0.1478449000
_diffrn_orient_matrix_UB_22      0.0227789000
_diffrn_orient_matrix_UB_23      -0.0866371000
_diffrn_orient_matrix_UB_31      -0.0805436000
_diffrn_orient_matrix_UB_32      -0.0715773000
_diffrn_orient_matrix_UB_33      0.0542252000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3286
_reflns_number_total             3408
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.461
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.089
_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)+(0.0322P)²+0.8492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0553
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11)
1.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.25745(2) 0.15696(2) 0.49374(2) 0.02780(6) Uani 1 1 d . . . . .
O3 O 0.5491(3) 0.16954(16) 0.7000(2) 0.0491(5) Uani 1 1 d . . . . .
O5 O -0.0395(3) 0.14444(16) 0.2919(2) 0.0537(6) Uani 1 1 d . . . . .
N1 N 0.2360(2) 0.37160(19) 0.50957(16) 0.0323(5) Uani 1 1 d . . . . .
O4 O 0.4426(3) 0.19171(18) 0.3017(2) 0.0580(6) Uani 1 1 d . . . . .
C8 C 0.1767(3) 0.50703(17) 0.5906(2) 0.0295(5) Uani 1 1 d . . . . .
C9 C 0.1768(3) 0.59848(17) 0.5863(2) 0.0318(5) Uani 1 1 d . . . . .
H9 H 0.135233 0.630612 0.639924 0.038 Uiso 1 1 calc R U . . .
C7 C 0.2376(2) 0.46338(18) 0.50958(19) 0.0295(5) Uani 1 1 d . . . . .
O1 O 0.3133(3) -0.04702(14) 0.4805(2) 0.0680(7) Uani 1 1 d . . . . .
C3 C 0.4461(4) 0.16519(17) 0.6256(3) 0.0353(6) Uani 1 1 d . . . . .
C10 C 0.2361(3) 0.6436(2) 0.5058(2) 0.0335(6) Uani 1 1 d . . . . .
C12 C 0.3007(3) 0.50523(17) 0.4276(2) 0.0290(5) Uani 1 1 d . . . . .
C6 C 0.2377(3) 0.2953(2) 0.50486(19) 0.0320(6) Uani 1 1 d . . . . .
C5 C 0.0668(4) 0.14954(17) 0.3642(3) 0.0376(6) Uani 1 1 d . . . . .
C4 C 0.3780(3) 0.1786(2) 0.3709(3) 0.0384(6) Uani 1 1 d . . . . .
O2 O 0.0568(3) 0.1227(2) 0.6746(2) 0.0769(8) Uani 1 1 d . . . . .
C15 C 0.3653(3) 0.45464(18) 0.3417(2) 0.0365(5) Uani 1 1 d . . . . .
H15A H 0.440553 0.413387 0.383585 0.055 Uiso 1 1 calc R U . . .
H15B H 0.411906 0.495419 0.296740 0.055 Uiso 1 1 calc R U . . .
H15C H 0.285577 0.422138 0.288915 0.055 Uiso 1 1 calc R U . . .
C11 C 0.2991(3) 0.59677(17) 0.4278(2) 0.0320(5) Uani 1 1 d . . . . .
H11 H 0.341806 0.627767 0.373848 0.038 Uiso 1 1 calc R U . . .
C13 C 0.1140(3) 0.45835(18) 0.6795(2) 0.0362(5) Uani 1 1 d . . . . .
H13A H 0.070877 0.500362 0.725195 0.054 Uiso 1 1 calc R U . . .
H13B H 0.193965 0.425348 0.731269 0.054 Uiso 1 1 calc R U . . .
H13C H 0.036242 0.417702 0.639681 0.054 Uiso 1 1 calc R U . . .
C1 C 0.2905(4) 0.0257(2) 0.4846(3) 0.0464(7) Uani 1 1 d . . . . .
C14 C 0.2315(3) 0.7430(2) 0.5016(2) 0.0446(7) Uani 1 1 d . . . . .
H14A H 0.132315 0.762363 0.459077 0.067 Uiso 1 1 calc R U . . .
H14B H 0.306822 0.764549 0.461949 0.067 Uiso 1 1 calc R U . . .
H14C H 0.252517 0.766307 0.581029 0.067 Uiso 1 1 calc R U . . .
C2 C 0.1300(3) 0.1360(2) 0.6113(3) 0.0435(6) Uani 1 1 d . . . . .


_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
W1 C3 2.049(3) . ?
W1 C6 2.124(3) . ?
W1 C5 2.045(3) . ?
W1 C4 2.051(3) . ?
W1 C1 2.032(3) . ?
W1 C2 2.043(3) . ?
O3 C3 1.135(4) . ?
O5 C5 1.142(4) . ?
N1 C7 1.399(4) . ?
N1 C6 1.165(5) . ?
O4 C4 1.136(4) . ?
C8 C9 1.395(4) . ?
C8 C7 1.387(3) . ?
C8 C13 1.507(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(4) . ?
C7 C12 1.396(3) . ?
O1 C1 1.131(4) . ?
C10 C11 1.395(4) . ?
C10 C14 1.516(5) . ?
C12 C15 1.504(3) . ?
C12 C11 1.396(4) . ?
O2 C2 1.136(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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
C3 W1 C6 87.81(9) . . ?
C3 W1 C4 91.46(12) . . ?
C5 W1 C3 178.94(10) . . ?
C5 W1 C6 91.74(9) . . ?
C5 W1 C4 89.48(12) . . ?
C4 W1 C6 87.29(10) . . ?
C1 W1 C3 89.42(11) . . ?
C1 W1 C6 176.37(11) . . ?
C1 W1 C5 91.07(11) . . ?
C1 W1 C4 90.44(13) . . ?
C1 W1 C2 89.97(14) . . ?
C2 W1 C3 90.69(12) . . ?
C2 W1 C6 92.40(12) . . ?
C2 W1 C5 88.37(12) . . ?
C2 W1 C4 177.82(10) . . ?
C6 N1 C7 176.7(2) . . ?
C9 C8 C13 121.4(2) . . ?
C7 C8 C9 116.8(2) . . ?
C7 C8 C13 121.8(2) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 C8 121.7(2) . . ?
C10 C9 H9 119.2 . . ?
C8 C7 N1 118.3(2) . . ?
C8 C7 C12 124.1(3) . . ?
C12 C7 N1 117.6(2) . . ?
O3 C3 W1 178.8(3) . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 C14 120.4(2) . . ?
C11 C10 C14 120.2(3) . . ?
C7 C12 C15 121.9(2) . . ?
C7 C12 C11 116.7(2) . . ?
C11 C12 C15 121.3(2) . . ?
N1 C6 W1 175.6(2) . . ?
O5 C5 W1 179.3(3) . . ?
O4 C4 W1 178.6(3) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C11 C12 121.3(2) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C1 W1 178.0(3) . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C2 W1 178.1(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
N1 C7 C12 C15 0.0(3) . . . . ?
N1 C7 C12 C11 179.0(2) . . . . ?
C8 C9 C10 C11 -0.8(3) . . . . ?
C8 C9 C10 C14 178.7(2) . . . . ?
C8 C7 C12 C15 179.9(2) . . . . ?
C8 C7 C12 C11 -1.0(3) . . . . ?
C9 C8 C7 N1 -178.5(2) . . . . ?
C9 C8 C7 C12 1.6(3) . . . . ?
C9 C10 C11 C12 1.4(3) . . . . ?
C7 C8 C9 C10 -0.6(4) . . . . ?
C7 C12 C11 C10 -0.6(3) . . . . ?
C15 C12 C11 C10 178.5(2) . . . . ?
C13 C8 C9 C10 179.2(2) . . . . ?
C13 C8 C7 N1 1.8(3) . . . . ?
C13 C8 C7 C12 -178.2(2) . . . . ?
C14 C10 C11 C12 -178.1(2) . . . . ?


_ins_header                      
;
TITL RMK_365_A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.212120  15.247762  11.819159  90.0000 103.5198  90.0000
ZERR    4.00   0.000084   0.000138   0.000105   0.0000   0.0010   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O W
UNIT 60.00 44.00 4.00 20.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.10 0.20 0.24
TREF
HKLF 4
END
;
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.755
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/hexane'
####################################################################### 
# 
# 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_rmk_344_scale
_database_code_depnum_ccdc_archive 'CCDC 2403975'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-09-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H18 Fe N O4 P'
_chemical_formula_sum            'C13 H18 Fe N O4 P'
_chemical_formula_weight         339.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C13H18Fe1O4N1P1 '
_chemical_oxdiff_usercomment     'pentane evap at -30 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   20.8819(5)
_cell_length_b                   10.0111(3)
_cell_length_c                   16.0053(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3345.92(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5114
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.4290
_cell_measurement_theta_min      4.2400
_shelx_estimated_absorpt_T_max   0.451
_shelx_estimated_absorpt_T_min   0.270
_exptl_absorpt_coefficient_mu    8.237
_exptl_absorpt_correction_T_max  0.38250
_exptl_absorpt_correction_T_min  0.30759
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
13 2 -2 0.1048
-13 -2 2 0.1048
3 -1 10 0.1062
-2 1 -10 0.0854
4 -6 -1 0.0573
-4 6 1 0.0573
-10 -5 -1 0.0738

_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.115
_exptl_crystal_size_rad          0.100
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.7240 1.8104 -2.1188 -0.3724 0.0116 -0.9280
-12.7240 -1.8104 2.1188 0.3724 -0.0116 0.9280
3.1541 -0.8726 10.0050 0.9332 -0.0225 -0.3585
-2.0981 1.0167 -10.1325 -0.9594 0.0234 0.2809
4.4629 -6.1197 -0.7343 0.0788 -0.9909 -0.1087
-4.4629 6.1197 0.7343 -0.0788 0.9909 0.1087
-9.6530 -4.5306 -0.7992 0.1550 -0.5127 0.8445

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.129
_diffrn_reflns_theta_min         4.234
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -72.00   0.50    1.00    --  -46.45 173.00-164.00   64
  2  ω    106.00 174.00   0.50   10.00    --  107.75  21.00 -34.00  136
  3  ω    110.00 166.00   0.50   10.00    --  107.75 110.00 149.00  112
  4  ω     67.00 147.00   0.50   10.00    --  107.75-173.00-175.00  160
  5  ω     -6.00  29.00   0.50    1.00    --  -46.45  19.00  60.00   70
  6  ω     -7.00  28.00   0.50    1.00    --  -46.45  19.00 -30.00   70
  7  ω     -1.00  25.00   0.50    1.00    --  -46.45  19.00-150.00   52
  8  ω    -20.00  22.00   0.50    1.00    --  -46.45  38.00-180.00   84
  9  ω     87.00 119.00   0.50    1.00    --   46.45 173.00-164.00   64
 10  ω     37.00  63.00   0.50   10.00    --  107.75 -45.00  30.00   52
 11  ω     32.00  57.00   0.50   10.00    --  107.75 -30.00-150.00   50
 12  ω     32.00  58.00   0.50   10.00    --  107.75 -30.00  30.00   52
 13  ω     36.00  61.00   0.50   10.00    --  107.75 -45.00 150.00   50
 14  ω     37.00  62.00   0.50   10.00    --  107.75 -45.00-120.00   50
 15  ω     75.00 101.00   0.50   10.00    --  107.75 -95.00   0.00   52
 16  ω     36.00  68.00   0.50   10.00    --  107.75 -45.00 120.00   64
 17  ω     34.00  59.00   0.50   10.00    --  107.75 -30.00  90.00   50
 18  ω     63.00  88.00   0.50   10.00    --  107.75 -61.00   0.00   50
 19  ω     33.00  58.00   0.50   10.00    --  107.75 -30.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0093009000
_diffrn_orient_matrix_UB_12      -0.0308805000
_diffrn_orient_matrix_UB_13      0.0935169000
_diffrn_orient_matrix_UB_21      -0.0173722000
_diffrn_orient_matrix_UB_22      0.1473305000
_diffrn_orient_matrix_UB_23      0.0160759000
_diffrn_orient_matrix_UB_31      -0.0710660000
_diffrn_orient_matrix_UB_32      -0.0321206000
_diffrn_orient_matrix_UB_33      -0.0162324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2781
_reflns_number_total             3503
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.062
_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)+(0.0837P)²+0.5220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1360
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe1 Fe 0.57050(2) 0.74940(4) 0.63290(2) 0.03309(16) Uani 1 1 d . . . . .
P1 P 0.69706(3) 0.35411(6) 0.63919(3) 0.03101(17) Uani 1 1 d . . . . .
O3 O 0.63392(11) 0.8286(2) 0.78927(12) 0.0533(5) Uani 1 1 d . . . . .
O1 O 0.48826(11) 0.9873(2) 0.63620(16) 0.0608(6) Uani 1 1 d . . . . .
O4 O 0.46014(11) 0.5667(3) 0.63904(15) 0.0602(6) Uani 1 1 d . . . . .
O2 O 0.62619(13) 0.8340(3) 0.47224(14) 0.0662(7) Uani 1 1 d . . . . .
N1 N 0.64934(10) 0.4957(2) 0.63447(13) 0.0376(5) Uani 1 1 d . . . . .
C10 C 0.66307(13) 0.2825(3) 0.73807(16) 0.0376(5) Uani 1 1 d . . . . .
C4 C 0.50187(13) 0.6398(3) 0.63659(16) 0.0422(6) Uani 1 1 d . . . . .
C6 C 0.66693(14) 0.2702(3) 0.54223(16) 0.0395(6) Uani 1 1 d . . . . .
C3 C 0.60929(13) 0.7988(3) 0.72820(17) 0.0398(5) Uani 1 1 d . . . . .
C5 C 0.62089(12) 0.5949(3) 0.63298(14) 0.0359(5) Uani 1 1 d . . . . .
C11 C 0.68652(14) 0.3781(3) 0.80621(16) 0.0441(6) Uani 1 1 d . . . . .
H11A H 0.733192 0.386765 0.802793 0.066 Uiso 1 1 calc R U . . .
H11B H 0.674656 0.342866 0.861197 0.066 Uiso 1 1 calc R U . . .
H11C H 0.666711 0.465957 0.798249 0.066 Uiso 1 1 calc R U . . .
C1 C 0.52000(13) 0.8944(3) 0.63467(16) 0.0418(6) Uani 1 1 d . . . . .
C7 C 0.68589(16) 0.3643(3) 0.47090(16) 0.0493(7) Uani 1 1 d . . . . .
H7A H 0.660730 0.446675 0.474644 0.074 Uiso 1 1 calc R U . . .
H7B H 0.677500 0.320590 0.417205 0.074 Uiso 1 1 calc R U . . .
H7C H 0.731563 0.385654 0.475224 0.074 Uiso 1 1 calc R U . . .
C2 C 0.60427(14) 0.8004(3) 0.53444(17) 0.0439(6) Uani 1 1 d . . . . .
C9 C 0.7067(2) 0.1417(3) 0.5316(2) 0.0640(9) Uani 1 1 d . . . . .
H9A H 0.752353 0.163532 0.534286 0.096 Uiso 1 1 calc R U . . .
H9B H 0.696903 0.100937 0.477445 0.096 Uiso 1 1 calc R U . . .
H9C H 0.695967 0.078838 0.576466 0.096 Uiso 1 1 calc R U . . .
C13 C 0.69558(19) 0.1463(3) 0.7507(2) 0.0598(9) Uani 1 1 d . . . . .
H13A H 0.680802 0.083908 0.707634 0.090 Uiso 1 1 calc R U . . .
H13B H 0.684552 0.111154 0.806037 0.090 Uiso 1 1 calc R U . . .
H13C H 0.742128 0.156836 0.746555 0.090 Uiso 1 1 calc R U . . .
C12 C 0.59015(16) 0.2706(4) 0.7441(2) 0.0550(8) Uani 1 1 d . . . . .
H12A H 0.570456 0.355546 0.727820 0.083 Uiso 1 1 calc R U . . .
H12B H 0.578021 0.248880 0.801637 0.083 Uiso 1 1 calc R U . . .
H12C H 0.575279 0.199665 0.706573 0.083 Uiso 1 1 calc R U . . .
C8 C 0.59557(18) 0.2407(4) 0.5370(2) 0.0634(10) Uani 1 1 d . . . . .
H8A H 0.584350 0.172151 0.578194 0.095 Uiso 1 1 calc R U . . .
H8B H 0.585052 0.208604 0.480845 0.095 Uiso 1 1 calc R U . . .
H8C H 0.571334 0.322465 0.548707 0.095 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
Fe1 C4 1.806(3) . ?
Fe1 C3 1.797(3) . ?
Fe1 C5 1.870(3) . ?
Fe1 C1 1.795(3) . ?
Fe1 C2 1.800(3) . ?
P1 N1 1.734(2) . ?
P1 C10 1.877(3) . ?
P1 C6 1.873(3) . ?
O3 C3 1.144(3) . ?
O1 C1 1.142(4) . ?
O4 C4 1.138(4) . ?
O2 C2 1.146(4) . ?
N1 C5 1.158(4) . ?
C10 C11 1.532(4) . ?
C10 C13 1.537(4) . ?
C10 C12 1.530(4) . ?
C6 C7 1.532(4) . ?
C6 C9 1.540(4) . ?
C6 C8 1.521(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
C4 Fe1 C5 86.80(12) . . ?
C3 Fe1 C4 119.83(12) . . ?
C3 Fe1 C5 88.48(11) . . ?
C3 Fe1 C2 119.23(13) . . ?
C1 Fe1 C4 91.42(12) . . ?
C1 Fe1 C3 91.64(12) . . ?
C1 Fe1 C5 178.01(11) . . ?
C1 Fe1 C2 90.83(12) . . ?
C2 Fe1 C4 120.79(13) . . ?
C2 Fe1 C5 90.84(11) . . ?
N1 P1 C10 97.57(11) . . ?
N1 P1 C6 97.89(11) . . ?
C6 P1 C10 113.59(13) . . ?
C5 N1 P1 175.6(2) . . ?
C11 C10 P1 103.92(17) . . ?
C11 C10 C13 108.6(2) . . ?
C13 C10 P1 106.44(19) . . ?
C12 C10 P1 117.3(2) . . ?
C12 C10 C11 108.8(2) . . ?
C12 C10 C13 111.2(3) . . ?
O4 C4 Fe1 177.4(3) . . ?
C7 C6 P1 104.78(18) . . ?
C7 C6 C9 107.0(3) . . ?
C9 C6 P1 106.54(19) . . ?
C8 C6 P1 117.5(2) . . ?
C8 C6 C7 109.4(2) . . ?
C8 C6 C9 111.1(3) . . ?
O3 C3 Fe1 179.1(3) . . ?
N1 C5 Fe1 176.4(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C1 Fe1 179.4(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C2 Fe1 179.2(3) . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
N1 P1 C10 C11 -70.07(19) . . . . ?
N1 P1 C10 C13 175.3(2) . . . . ?
N1 P1 C10 C12 50.0(2) . . . . ?
N1 P1 C6 C7 63.9(2) . . . . ?
N1 P1 C6 C9 177.1(2) . . . . ?
N1 P1 C6 C8 -57.7(2) . . . . ?
C10 P1 C6 C7 165.77(18) . . . . ?
C10 P1 C6 C9 -81.0(2) . . . . ?
C10 P1 C6 C8 44.2(3) . . . . ?
C6 P1 C10 C11 -172.14(17) . . . . ?
C6 P1 C10 C13 73.2(2) . . . . ?
C6 P1 C10 C12 -52.0(3) . . . . ?


_ins_header                      
;
TITL RMK_344_scale in Pbcn 
REM Pbcn (#60, found as Pbna in cab setting)
CELL 1.54184  20.881942  10.011102  16.005318  90.0000  90.0000  90.0000
ZERR    8.00   0.000491   0.000261   0.000351   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z+1/2 
SYMM -x, y,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N O P Fe
UNIT 104.00 144.00 8.00 32.00 8.00 8.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=300.0; aver:225.0
TEMP -48
SIZE 0.11 0.21 0.21
TREF
HKLF 4
END
;
_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 2.928
_oxdiff_exptl_absorpt_empirical_full_min 0.451
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_353_scale
_database_code_depnum_ccdc_archive 'CCDC 2403979'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-04-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 N O5 P W'
_chemical_formula_sum            'C14 H18 N O5 P W'
_chemical_formula_weight         495.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H18W1N1P1O5
_chemical_oxdiff_usercomment     'pentane evap'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   22.1015(3)
_cell_length_b                   13.5912(2)
_cell_length_c                   5.92670(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1780.30(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14426
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      77.5270
_cell_measurement_theta_min      3.9560
_shelx_estimated_absorpt_T_max   0.780
_shelx_estimated_absorpt_T_min   0.132
_exptl_absorpt_coefficient_mu    13.064
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -9 0 0.0475
1 9 0 0.0475
1 0 -4 0.1293
-1 0 4 0.1293
-14 2 0 0.0095
14 -2 0 0.0095

_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0865 -8.7976 0.0371 -0.6875 -0.7261 -0.0089
1.0865 8.7976 -0.0371 0.6875 0.7261 0.0089
0.7881 -0.3824 -3.8381 -0.0160 -0.0130 -0.9998
-0.7881 0.3824 3.8381 0.0160 0.0130 0.9998
-14.0905 1.5800 -0.2051 -0.6503 0.7597 0.0094
14.0905 -1.5800 0.2051 0.6503 -0.7597 -0.0094

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            21172
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.082
_diffrn_reflns_theta_min         4.000
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  24.00   0.50    0.50    --  -46.45  19.00-180.00   52
  2  ω     -1.00  25.00   0.50    0.50    --  -46.45  19.00   0.00   52
  3  ω    -43.00   1.00   0.50    0.50    --  -46.45  57.00 -60.00   88
  4  ω    -19.00  22.00   0.50    0.50    --  -46.45  38.00 150.00   82
  5  ω   -119.00  24.00   0.50    0.50    --  -46.45   0.00 -30.00  286
  6  ω     39.00  93.00   0.50    0.50    --   46.45-125.00  60.00  108
  7  ω     49.00  78.00   0.50    0.50    --   46.45-125.00-150.00   58
  8  ω    117.00 176.00   0.50    2.00    --  107.75  15.00 -60.00  118
  9  ω     33.00  59.00   0.50    2.00    --  107.75 -30.00 120.00   52
 10  ω     94.00 125.00   0.50    2.00    --  107.75-141.00-179.35   62
 11  ω     36.00  91.00   0.50    2.00    --  107.75 -95.00  30.00  110
 12  ω     48.00  73.00   0.50    2.00    --  107.75 -61.00 120.00   50
 13  ω     32.00  59.00   0.50    2.00    --  107.75 -30.00  30.00   54
 14  ω    104.00 175.00   0.50    2.00    --  107.75  30.00   0.00  142
 15  ω     32.00  57.00   0.50    2.00    --  107.75 -30.00 -60.00   50
 16  ω     49.00 110.00   0.50    2.00    --  107.75-125.00   0.00  122
 17  ω     35.00  92.00   0.50    2.00    --  107.75 -61.00-150.00  114
 18  ω     79.00 108.00   0.50    2.00    --  107.75-107.00-126.09   58
 19  ω     84.00 109.00   0.50    2.00    --  107.75-111.00-172.38   50
 20  ω     39.00  68.00   0.50    2.00    --  107.75 -45.00  60.00   58
 21  ω    140.00 178.00   0.50    2.00    --  107.75 125.00 -60.00   76
 22  ω     39.00  65.00   0.50    2.00    --  107.75 -45.00-150.00   52
 23  ω     37.00  65.00   0.50    2.00    --  107.75-107.00-126.09   56
 24  ω     37.00  70.00   0.50    2.00    --  107.75 -95.00 150.00   66
 25  ω     79.00 104.00   0.50    2.00    --  107.75 -95.00 150.00   50
 26  ω    104.00 159.00   0.50    2.00    --  107.75  30.00-150.00  110
 27  ω     95.00 146.00   0.50    2.00    --  107.75 125.00  90.00  102
 28  ω     53.00  90.00   0.50    2.00    --  107.75 -95.00  90.00   74
 29  ω     53.00 103.00   0.50    2.00    --  107.75 -95.00-150.00  100
 30  ω     45.00  75.00   0.50    2.00    --  107.75 -61.00 -30.00   60
 31  ω     59.00 104.00   0.50    2.00    --  107.75 -95.00 -90.00   90
 32  ω     95.00 131.00   0.50    2.00    --  107.75  45.00  60.00   72
 33  ω     37.00  73.00   0.50    2.00    --  107.75 -45.00-120.00   72
 34  ω    103.00 129.00   0.50    2.00    --  107.75 125.00 -60.00   52
 35  ω     45.00  72.00   0.50    2.00    --  107.75 -45.00 -30.00   54
 36  ω     83.00 108.00   0.50    2.00    --  107.75-110.00  81.01   50
 37  ω     78.00 104.00   0.50    2.00    --  107.75 -95.00   0.00   52
 38  ω     42.00  68.00   0.50    2.00    --  107.75-111.00-172.38   52
 39  ω     42.00  83.00   0.50    2.00    --  107.75-141.00-179.35   82
 40  ω     96.00 175.00   0.50    2.00    --  107.75  15.00 -90.00  158
 41  ω     42.00  67.00   0.50    2.00    --  107.75 -45.00 -90.00   50
 42  ω     35.00 106.00   0.50    2.00    --  107.75 -95.00  60.00  142
 43  ω     69.00 108.00   0.50    2.00    --  107.75-104.00 -17.11   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0540484000
_diffrn_orient_matrix_UB_12      0.0715095000
_diffrn_orient_matrix_UB_13      0.0081543000
_diffrn_orient_matrix_UB_21      -0.0438485000
_diffrn_orient_matrix_UB_22      0.0878884000
_diffrn_orient_matrix_UB_23      -0.0143791000
_diffrn_orient_matrix_UB_31      -0.0041498000
_diffrn_orient_matrix_UB_32      0.0026227000
_diffrn_orient_matrix_UB_33      0.2593790000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1831
_reflns_number_total             1978
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.052
_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)+(0.0694P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.19898(2) 0.250000 0.47232(4) 0.02750(13) Uani 1 2 d S T P . .
P1 P 0.39784(4) 0.250000 0.87518(15) 0.0230(2) Uani 1 2 d S T P . .
O2 O 0.14629(13) 0.4100(2) 0.8114(5) 0.0461(6) Uani 1 1 d . . . . .
O1 O 0.07811(17) 0.250000 0.1867(7) 0.0489(9) Uani 1 2 d S T P . .
C5 C 0.42938(16) 0.3645(2) 0.7453(5) 0.0281(6) Uani 1 1 d . . . . .
C1 C 0.1220(2) 0.250000 0.2895(8) 0.0355(10) Uani 1 2 d S T P . .
C4 C 0.2821(2) 0.250000 0.6505(8) 0.0277(8) Uani 1 2 d S T P . .
O3 O 0.25428(14) 0.0815(2) 0.1595(6) 0.0574(8) Uani 1 1 d . . . . .
N1 N 0.32919(18) 0.250000 0.7352(7) 0.0306(8) Uani 1 2 d S T P . .
C2 C 0.16511(15) 0.3542(3) 0.6889(6) 0.0331(7) Uani 1 1 d . . . . .
C7 C 0.4282(2) 0.3721(3) 0.4886(6) 0.0446(10) Uani 1 1 d . . . . .
H7A H 0.457016 0.325058 0.424180 0.067 Uiso 1 1 calc R U . . .
H7B H 0.439344 0.438950 0.442994 0.067 Uiso 1 1 calc R U . . .
H7C H 0.387378 0.357053 0.433685 0.067 Uiso 1 1 calc R U . . .
C6 C 0.39047(17) 0.4477(3) 0.8436(7) 0.0399(7) Uani 1 1 d . . . . .
H6A H 0.349433 0.443463 0.781776 0.060 Uiso 1 1 calc R U . . .
H6B H 0.408302 0.511356 0.803615 0.060 Uiso 1 1 calc R U . . .
H6C H 0.388855 0.441327 1.008218 0.060 Uiso 1 1 calc R U . . .
C3 C 0.23473(16) 0.1421(3) 0.2680(6) 0.0373(7) Uani 1 1 d . . . . .
C8 C 0.49438(17) 0.3759(3) 0.8335(8) 0.0445(8) Uani 1 1 d . . . . .
H8A H 0.495181 0.362934 0.996118 0.067 Uiso 1 1 calc R U . . .
H8B H 0.508568 0.443006 0.804540 0.067 Uiso 1 1 calc R U . . .
H8C H 0.520850 0.328912 0.755990 0.067 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
W1 C1 2.018(5) . ?
W1 C4 2.119(4) . ?
W1 C2 2.053(4) 7_565 ?
W1 C2 2.053(4) . ?
W1 C3 2.059(4) 7_565 ?
W1 C3 2.059(4) . ?
P1 C5 1.871(3) . ?
P1 C5 1.871(3) 7_565 ?
P1 N1 1.729(4) . ?
O2 C2 1.129(5) . ?
O1 C1 1.145(6) . ?
C5 C7 1.525(4) . ?
C5 C6 1.535(4) . ?
C5 C8 1.537(4) . ?
C4 N1 1.156(6) . ?
O3 C3 1.131(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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 W1 C4 177.42(19) . . ?
C1 W1 C2 91.61(14) . . ?
C1 W1 C2 91.61(14) . 7_565 ?
C1 W1 C3 90.45(13) . . ?
C1 W1 C3 90.45(13) . 7_565 ?
C2 W1 C4 90.26(13) 7_565 . ?
C2 W1 C4 90.26(13) . . ?
C2 W1 C2 87.22(19) . 7_565 ?
C2 W1 C3 177.28(13) 7_565 7_565 ?
C2 W1 C3 90.95(15) 7_565 . ?
C2 W1 C3 177.28(13) . . ?
C2 W1 C3 90.95(15) . 7_565 ?
C3 W1 C4 87.74(13) 7_565 . ?
C3 W1 C4 87.74(13) . . ?
C3 W1 C3 90.8(2) 7_565 . ?
C5 P1 C5 112.6(2) . 7_565 ?
N1 P1 C5 97.44(13) . . ?
N1 P1 C5 97.44(13) . 7_565 ?
C7 C5 P1 117.4(2) . . ?
C7 C5 C6 108.6(3) . . ?
C7 C5 C8 110.4(3) . . ?
C6 C5 P1 104.3(2) . . ?
C6 C5 C8 108.7(3) . . ?
C8 C5 P1 107.0(2) . . ?
O1 C1 W1 179.7(4) . . ?
N1 C4 W1 175.8(4) . . ?
C4 N1 P1 177.1(4) . . ?
O2 C2 W1 178.6(3) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C3 W1 178.5(3) . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
C5 P1 C5 C7 50.2(4) 7_565 . . . ?
C5 P1 C5 C6 170.47(16) 7_565 . . . ?
C5 P1 C5 C8 -74.4(3) 7_565 . . . ?
N1 P1 C5 C7 -51.0(3) . . . . ?
N1 P1 C5 C6 69.2(3) . . . . ?
N1 P1 C5 C8 -175.7(3) . . . . ?


_ins_header                      
;
TITL RMK_353_scale in Pnma 
REM Pnma (#62, found as Pcmn in -cba setting)
CELL 1.54184  22.101511  13.591167   5.926654  90.0000  90.0000  90.0000
ZERR    4.00   0.000255   0.000167   0.000052   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y+1/2,-z+1/2 
SFAC C H N O P W
UNIT 56.00 72.00 4.00 20.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.02 0.10 0.26
TREF
HKLF 4
END
;
_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 2.101
_oxdiff_exptl_absorpt_empirical_full_min 0.511
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: benzene'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_377_b_scale
_database_code_depnum_ccdc_archive 'CCDC 2403971'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H23 Mn N O2 P'
_chemical_formula_sum            'C16 H23 Mn N O2 P'
_chemical_formula_weight         347.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H23Mn1N1O2P1
_chemical_oxdiff_usercomment     'hexane evap at -30 '
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3531(6)
_cell_length_b                   6.3326(3)
_cell_length_c                   26.3915(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.390(5)
_cell_angle_gamma                90
_cell_volume                     1729.77(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4572
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.9180
_cell_measurement_theta_min      2.5430
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.747
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -4 34 0.0810
1 -4 -34 0.1001
-1 9 4 0.1164
15 0 -2 0.0513
-15 1 -2 0.0296
-2 8 -18 0.1007
-13 -2 -13 0.0590

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.2867 -3.8118 33.6167 -0.0542 0.0285 0.9981
0.6472 -3.7387 -33.7700 -0.6578 0.3111 -0.6860
-1.1148 8.8573 3.7030 0.8671 -0.4132 -0.2783
14.5863 -0.1540 -2.1951 -0.5216 -0.8532 -0.0093
-14.5347 0.5352 -1.7753 0.5189 0.8483 -0.1055
-1.8682 7.6969 -18.1300 0.5941 -0.2078 -0.7771
-13.0860 -2.1994 -12.9288 0.1254 0.9556 -0.2665

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.888
_diffrn_reflns_theta_min         2.472
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  16.00   0.50    2.00    --   -4.70  29.00-126.00   64
  2  ω    -68.00   4.00   0.50    2.00    --   -4.70 -29.00  71.00  144
  3  ω    -24.00  35.00   0.50    2.00    --    1.66 -99.00-180.00  118
  4  ω     -9.00  75.00   0.50    2.00    --    1.66  38.00 -30.00  168
  5  ω    -72.00  16.00   0.50    2.00    --    1.66 -38.00-180.00  176
  6  ω    -51.00 -26.00   0.50    2.00    --    1.66 -38.00  30.00   50
  7  ω     -6.00  26.00   0.50    2.00    --   -4.70 -99.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334727000
_diffrn_orient_matrix_UB_12      0.0899693000
_diffrn_orient_matrix_UB_13      0.0088756000
_diffrn_orient_matrix_UB_21      -0.0597294000
_diffrn_orient_matrix_UB_22      -0.0522605000
_diffrn_orient_matrix_UB_23      -0.0045701000
_diffrn_orient_matrix_UB_31      0.0026814000
_diffrn_orient_matrix_UB_32      -0.0415143000
_diffrn_orient_matrix_UB_33      0.0249612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3226
_reflns_number_total             4339
_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 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.020
_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)+(0.0313P)²+1.1099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1017
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C14(H14), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C9(H9a,H9b,H9c), C7(H7a,H7b,H7c), C10(H10a,H10b,H10c),
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Mn1 Mn 0.40094(3) 0.56526(5) 0.40528(2) 0.01828(11) Uani 1 1 d . . . . .
P1 P 0.76629(6) 0.18216(10) 0.35994(2) 0.02229(15) Uani 1 1 d . . . . .
O2 O 0.28207(19) 0.2906(3) 0.48078(7) 0.0325(4) Uani 1 1 d . . . . .
O1 O 0.2740(2) 0.3444(3) 0.31976(7) 0.0395(5) Uani 1 1 d . . . . .
N1 N 0.6495(2) 0.3277(3) 0.38893(8) 0.0246(4) Uani 1 1 d . . . . .
C3 C 0.5507(2) 0.4135(4) 0.39622(8) 0.0213(5) Uani 1 1 d . . . . .
C15 C 0.4168(3) 0.8181(4) 0.45916(9) 0.0272(5) Uani 1 1 d . . . . .
H15 H 0.427120 0.798785 0.494724 0.033 Uiso 1 1 calc R U . . .
C16 C 0.2971(3) 0.8332(4) 0.43154(9) 0.0275(5) Uani 1 1 d . . . . .
H16 H 0.213353 0.825128 0.445339 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3326(2) 0.3920(4) 0.45069(9) 0.0228(5) Uani 1 1 d . . . . .
C14 C 0.5171(3) 0.8370(4) 0.42432(10) 0.0292(6) Uani 1 1 d . . . . .
H14 H 0.606985 0.832503 0.432367 0.035 Uiso 1 1 calc R U . . .
C1 C 0.3241(2) 0.4298(4) 0.35358(9) 0.0246(5) Uani 1 1 d . . . . .
C12 C 0.3256(3) 0.8623(4) 0.37995(10) 0.0279(6) Uani 1 1 d . . . . .
H12 H 0.263965 0.878135 0.352957 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4611(3) 0.8640(4) 0.37529(10) 0.0282(6) Uani 1 1 d . . . . .
H13 H 0.506617 0.880204 0.344708 0.034 Uiso 1 1 calc R U . . .
C8 C 0.9099(2) 0.2628(4) 0.39969(9) 0.0275(5) Uani 1 1 d . . . . .
C11 C 1.0232(3) 0.1254(5) 0.38329(13) 0.0424(7) Uani 1 1 d . . . . .
H11A H 0.997783 -0.023651 0.384037 0.064 Uiso 1 1 calc R U . . .
H11B H 1.097198 0.147813 0.406529 0.064 Uiso 1 1 calc R U . . .
H11C H 1.047162 0.164013 0.348809 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7620(3) 0.3172(5) 0.29656(10) 0.0368(7) Uani 1 1 d . . . . .
C9 C 0.8767(3) 0.2042(7) 0.45405(11) 0.0557(10) Uani 1 1 d . . . . .
H9A H 0.807451 0.296441 0.465727 0.084 Uiso 1 1 calc R U . . .
H9B H 0.953364 0.221769 0.476140 0.084 Uiso 1 1 calc R U . . .
H9C H 0.847900 0.056869 0.455118 0.084 Uiso 1 1 calc R U . . .
C7 C 0.8769(3) 0.2345(6) 0.26615(11) 0.0506(9) Uani 1 1 d . . . . .
H7A H 0.957576 0.292518 0.280444 0.076 Uiso 1 1 calc R U . . .
H7B H 0.866563 0.278362 0.230675 0.076 Uiso 1 1 calc R U . . .
H7C H 0.879443 0.079953 0.268013 0.076 Uiso 1 1 calc R U . . .
C10 C 0.9494(4) 0.4954(5) 0.39834(15) 0.0571(9) Uani 1 1 d . . . . .
H10A H 0.978748 0.531258 0.364375 0.086 Uiso 1 1 calc R U . . .
H10B H 1.019627 0.520236 0.423184 0.086 Uiso 1 1 calc R U . . .
H10C H 0.875108 0.583843 0.406583 0.086 Uiso 1 1 calc R U . . .
C5 C 0.6361(3) 0.2314(8) 0.27143(12) 0.0633(11) Uani 1 1 d . . . . .
H5A H 0.640932 0.077167 0.269084 0.095 Uiso 1 1 calc R U . . .
H5B H 0.625305 0.291415 0.237366 0.095 Uiso 1 1 calc R U . . .
H5C H 0.562274 0.271258 0.291925 0.095 Uiso 1 1 calc R U . . .
C6 C 0.7590(5) 0.5563(6) 0.29663(14) 0.0692(12) Uani 1 1 d . . . . .
H6A H 0.692646 0.605478 0.319718 0.104 Uiso 1 1 calc R U . . .
H6B H 0.738834 0.607426 0.262290 0.104 Uiso 1 1 calc R U . . .
H6C H 0.843501 0.610645 0.307912 0.104 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
Mn1 C3 1.845(2) . ?
Mn1 C15 2.145(2) . ?
Mn1 C16 2.133(2) . ?
Mn1 C2 1.784(3) . ?
Mn1 C14 2.152(3) . ?
Mn1 C1 1.783(3) . ?
Mn1 C12 2.138(2) . ?
Mn1 C13 2.148(2) . ?
P1 N1 1.715(2) . ?
P1 C8 1.870(3) . ?
P1 C4 1.878(3) . ?
O2 C2 1.156(3) . ?
O1 C1 1.156(3) . ?
N1 C3 1.178(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.426(4) . ?
C15 C14 1.408(4) . ?
C16 H16 0.9500 . ?
C16 C12 1.412(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.415(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.412(4) . ?
C13 H13 0.9500 . ?
C8 C11 1.532(4) . ?
C8 C9 1.529(4) . ?
C8 C10 1.530(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C4 C7 1.542(4) . ?
C4 C5 1.547(5) . ?
C4 C6 1.514(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
C3 Mn1 C15 115.06(10) . . ?
C3 Mn1 C16 152.65(11) . . ?
C3 Mn1 C14 88.86(10) . . ?
C3 Mn1 C12 136.01(10) . . ?
C3 Mn1 C13 99.13(10) . . ?
C15 Mn1 C14 38.26(10) . . ?
C15 Mn1 C13 64.45(10) . . ?
C16 Mn1 C15 38.93(10) . . ?
C16 Mn1 C14 64.61(10) . . ?
C16 Mn1 C12 38.61(10) . . ?
C16 Mn1 C13 64.68(10) . . ?
C2 Mn1 C3 96.60(10) . . ?
C2 Mn1 C15 92.24(10) . . ?
C2 Mn1 C16 93.43(10) . . ?
C2 Mn1 C14 124.30(10) . . ?
C2 Mn1 C12 127.14(11) . . ?
C2 Mn1 C13 155.83(10) . . ?
C1 Mn1 C3 90.62(11) . . ?
C1 Mn1 C15 153.16(11) . . ?
C1 Mn1 C16 114.37(11) . . ?
C1 Mn1 C2 92.37(11) . . ?
C1 Mn1 C14 143.14(10) . . ?
C1 Mn1 C12 91.81(11) . . ?
C1 Mn1 C13 105.65(11) . . ?
C12 Mn1 C15 64.65(10) . . ?
C12 Mn1 C14 64.33(10) . . ?
C12 Mn1 C13 38.46(10) . . ?
C13 Mn1 C14 38.43(10) . . ?
N1 P1 C8 99.35(11) . . ?
N1 P1 C4 98.68(11) . . ?
C8 P1 C4 112.14(13) . . ?
C3 N1 P1 160.9(2) . . ?
N1 C3 Mn1 175.7(2) . . ?
Mn1 C15 H15 124.3 . . ?
C16 C15 Mn1 70.09(13) . . ?
C16 C15 H15 126.1 . . ?
C14 C15 Mn1 71.13(14) . . ?
C14 C15 H15 126.1 . . ?
C14 C15 C16 107.8(2) . . ?
Mn1 C16 H16 123.6 . . ?
C15 C16 Mn1 70.98(14) . . ?
C15 C16 H16 126.2 . . ?
C12 C16 Mn1 70.85(14) . . ?
C12 C16 C15 107.6(2) . . ?
C12 C16 H16 126.2 . . ?
O2 C2 Mn1 175.2(2) . . ?
Mn1 C14 H14 124.5 . . ?
C15 C14 Mn1 70.61(14) . . ?
C15 C14 H14 125.8 . . ?
C15 C14 C13 108.4(2) . . ?
C13 C14 Mn1 70.65(14) . . ?
C13 C14 H14 125.8 . . ?
O1 C1 Mn1 179.1(2) . . ?
Mn1 C12 H12 124.1 . . ?
C16 C12 Mn1 70.53(14) . . ?
C16 C12 H12 125.8 . . ?
C13 C12 Mn1 71.19(14) . . ?
C13 C12 C16 108.4(2) . . ?
C13 C12 H12 125.8 . . ?
Mn1 C13 H13 124.2 . . ?
C14 C13 Mn1 70.92(14) . . ?
C14 C13 H13 126.1 . . ?
C12 C13 Mn1 70.35(14) . . ?
C12 C13 C14 107.8(2) . . ?
C12 C13 H13 126.1 . . ?
C11 C8 P1 106.89(19) . . ?
C9 C8 P1 105.45(19) . . ?
C9 C8 C11 108.6(2) . . ?
C9 C8 C10 108.8(3) . . ?
C10 C8 P1 117.3(2) . . ?
C10 C8 C11 109.5(2) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C4 P1 107.9(2) . . ?
C7 C4 C5 108.1(3) . . ?
C5 C4 P1 102.9(2) . . ?
C6 C4 P1 117.0(2) . . ?
C6 C4 C7 110.9(3) . . ?
C6 C4 C5 109.5(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
Mn1 C15 C16 C12 -61.75(17) . . . . ?
Mn1 C15 C14 C13 60.86(18) . . . . ?
Mn1 C16 C12 C13 -61.43(18) . . . . ?
Mn1 C14 C13 C12 61.02(18) . . . . ?
Mn1 C12 C13 C14 -61.38(17) . . . . ?
N1 P1 C8 C11 173.11(19) . . . . ?
N1 P1 C8 C9 57.7(2) . . . . ?
N1 P1 C8 C10 -63.6(2) . . . . ?
N1 P1 C4 C7 170.9(2) . . . . ?
N1 P1 C4 C5 -75.0(2) . . . . ?
N1 P1 C4 C6 45.1(3) . . . . ?
C15 C16 C12 Mn1 61.83(17) . . . . ?
C15 C16 C12 C13 0.4(3) . . . . ?
C15 C14 C13 Mn1 -60.83(18) . . . . ?
C15 C14 C13 C12 0.2(3) . . . . ?
C16 C15 C14 Mn1 -60.80(17) . . . . ?
C16 C15 C14 C13 0.1(3) . . . . ?
C16 C12 C13 Mn1 61.01(17) . . . . ?
C16 C12 C13 C14 -0.4(3) . . . . ?
C14 C15 C16 Mn1 61.47(17) . . . . ?
C14 C15 C16 C12 -0.3(3) . . . . ?
C8 P1 N1 C3 164.1(6) . . . . ?
C8 P1 C4 C7 67.1(2) . . . . ?
C8 P1 C4 C5 -178.8(2) . . . . ?
C8 P1 C4 C6 -58.7(3) . . . . ?
C4 P1 N1 C3 49.8(6) . . . . ?
C4 P1 C8 C11 -83.5(2) . . . . ?
C4 P1 C8 C9 161.1(2) . . . . ?
C4 P1 C8 C10 39.8(3) . . . . ?


_ins_header                      
;
TITL RMK_377_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  10.353067   6.332631  26.391526  90.0000  91.3904  90.0000
ZERR    4.00   0.000567   0.000342   0.001268   0.0000   0.0046   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O P Mn
UNIT 64.00 92.00 4.00 8.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.09 0.23 0.36
TREF
HKLF 4
END
;
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.734
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_376_b_scale
_database_code_depnum_ccdc_archive 'CCDC 2403974'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H33 Fe N O3 P2, C3 H7'
_chemical_formula_sum            'C33 H40 Fe N O3 P2'
_chemical_formula_weight         616.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         C33H40Fe1N1P2O3
_chemical_oxdiff_usercomment     'DCM/hexane evap at -30 '
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.9002(17)
_cell_length_b                   10.5291(9)
_cell_length_c                   18.4283(19)
_cell_angle_alpha                90
_cell_angle_beta                 110.203(12)
_cell_angle_gamma                90
_cell_volume                     3259.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9154
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.9680
_cell_measurement_theta_min      3.8630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-23 -1 0 0.1219
23 1 1 0.0846
-10 -3 25 0.3696
10 3 -25 0.4224
-2 14 -5 0.1193
6 -14 -3 0.1129
-11 10 19 0.2251
-13 -12 -4 0.1004
-15 11 -4 0.1243
16 -10 2 0.0949

_exptl_crystal_size_max          0.807
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.212
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-23.4879 -1.3387 -0.2738 0.7232 -0.6862 -0.0775
23.2784 1.2626 0.8916 -0.7244 0.6873 0.0533
-10.4383 -3.2236 25.2759 0.0100 -0.0097 -0.9999
10.0462 3.2051 -25.3169 0.0026 -0.0022 1.0000
-2.0302 14.4188 -4.7745 0.7040 0.6016 0.3773
5.5806 -14.4556 -3.3336 -0.7584 -0.6479 -0.0715
-10.9317 9.9775 18.5171 0.6284 0.5364 -0.5633
-12.7264 -11.6044 -4.4095 -0.0261 -0.9987 -0.0440
-14.9150 10.5005 -4.1592 0.9624 0.0757 0.2607
16.1059 -10.4202 1.9889 -0.9812 -0.0772 -0.1768

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34437
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.614
_diffrn_reflns_theta_min         3.569
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  31.00   1.00   10.00    --   -9.57 -99.00  90.00   46
  2  ω    -63.00  38.00   1.00   10.00    --    9.73 -57.00  60.00  101
  3  ω    -65.00  34.00   1.00   10.00    --    9.73 -37.00 -90.00   99
  4  ω    -23.00  12.00   1.00   10.00    --    9.73  77.00-120.00   35
  5  ω    -65.00  34.00   1.00   10.00    --    9.73 -37.00 150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0330661000
_diffrn_orient_matrix_UB_12      0.0415352000
_diffrn_orient_matrix_UB_13      -0.0079643000
_diffrn_orient_matrix_UB_21      0.0261129000
_diffrn_orient_matrix_UB_22      0.0510000000
_diffrn_orient_matrix_UB_23      0.0169059000
_diffrn_orient_matrix_UB_31      0.0029016000
_diffrn_orient_matrix_UB_32      0.0144855000
_diffrn_orient_matrix_UB_33      -0.0365138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5590
_reflns_number_total             7761
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.076
_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     368
_refine_ls_number_reflns         7761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      1.046
_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)+(0.0506P)²+3.6031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1348
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C20(H20), C26(H26), C14(H14), C18(H18), C24(H24), C22(H22),
 C17(H17), C28(H28), C21(H21), C29(H29), C27(H27), C16(H16), C15(H15), C23(H23)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe1 Fe 0.27956(2) 0.26744(4) 0.78357(2) 0.02421(11) Uani 1 1 d . . . . .
P2 P 0.36461(4) 0.40237(6) 0.76095(4) 0.02125(15) Uani 1 1 d . . . . .
P1 P 0.10466(4) -0.03057(7) 0.82915(4) 0.02905(17) Uani 1 1 d . . . . .
O2 O 0.40763(13) 0.0789(2) 0.82651(14) 0.0462(6) Uani 1 1 d . . . . .
O3 O 0.16161(13) 0.2893(2) 0.62757(13) 0.0480(6) Uani 1 1 d . . . . .
O1 O 0.25424(15) 0.4432(2) 0.89639(14) 0.0518(6) Uani 1 1 d . . . . .
N1 N 0.17143(14) 0.0780(2) 0.81850(14) 0.0341(5) Uani 1 1 d . . . . .
C19 C 0.46575(14) 0.3919(2) 0.83182(14) 0.0227(5) Uani 1 1 d . . . . .
C25 C 0.37990(14) 0.3880(3) 0.66811(14) 0.0243(5) Uani 1 1 d . . . . .
C13 C 0.33900(15) 0.5692(2) 0.76432(15) 0.0249(5) Uani 1 1 d . . . . .
C4 C 0.21325(16) 0.1510(3) 0.80501(15) 0.0280(6) Uani 1 1 d . . . . .
C30 C 0.37387(16) 0.2693(3) 0.63339(16) 0.0312(6) Uani 1 1 d . . . . .
H30 H 0.359550 0.198892 0.656124 0.037 Uiso 1 1 calc R U . . .
C20 C 0.47540(17) 0.3782(3) 0.90955(15) 0.0324(6) Uani 1 1 d . . . . .
H20 H 0.430789 0.374082 0.924375 0.039 Uiso 1 1 calc R U . . .
C3 C 0.20974(17) 0.2821(3) 0.68787(18) 0.0324(6) Uani 1 1 d . . . . .
C2 C 0.35727(16) 0.1523(3) 0.80869(17) 0.0314(6) Uani 1 1 d . . . . .
C26 C 0.40048(16) 0.4920(3) 0.63292(15) 0.0292(6) Uani 1 1 d . . . . .
H26 H 0.404333 0.571971 0.655396 0.035 Uiso 1 1 calc R U . . .
C14 C 0.26241(17) 0.6085(3) 0.71952(18) 0.0360(7) Uani 1 1 d . . . . .
H14 H 0.227062 0.550647 0.687292 0.043 Uiso 1 1 calc R U . . .
C18 C 0.39083(17) 0.6567(3) 0.81147(15) 0.0289(6) Uani 1 1 d . . . . .
H18 H 0.442368 0.632244 0.840801 0.035 Uiso 1 1 calc R U . . .
C24 C 0.53275(16) 0.3967(3) 0.81115(17) 0.0386(7) Uani 1 1 d . . . . .
H24 H 0.527627 0.405869 0.759458 0.046 Uiso 1 1 calc R U . . .
C22 C 0.61645(18) 0.3752(3) 0.94399(17) 0.0391(7) Uani 1 1 d . . . . .
H22 H 0.666971 0.369629 0.981339 0.047 Uiso 1 1 calc R U . . .
C1 C 0.26501(17) 0.3753(3) 0.85242(17) 0.0338(6) Uani 1 1 d . . . . .
C17 C 0.3665(2) 0.7803(3) 0.81531(17) 0.0395(7) Uani 1 1 d . . . . .
H17 H 0.401488 0.838358 0.847778 0.047 Uiso 1 1 calc R U . . .
C28 C 0.40949(18) 0.3592(3) 0.53090(16) 0.0400(7) Uani 1 1 d . . . . .
H28 H 0.419408 0.349578 0.484883 0.048 Uiso 1 1 calc R U . . .
C9 C 0.01493(17) 0.0751(3) 0.80142(19) 0.0385(7) Uani 1 1 d . . . . .
C21 C 0.55021(18) 0.3707(3) 0.96487(17) 0.0372(7) Uani 1 1 d . . . . .
H21 H 0.555737 0.362619 1.016724 0.045 Uiso 1 1 calc R U . . .
C29 C 0.38910(18) 0.2557(3) 0.56518(17) 0.0376(7) Uani 1 1 d . . . . .
H29 H 0.385502 0.176001 0.542455 0.045 Uiso 1 1 calc R U . . .
C27 C 0.41533(17) 0.4775(3) 0.56436(17) 0.0368(7) Uani 1 1 d . . . . .
H27 H 0.429218 0.547502 0.540983 0.044 Uiso 1 1 calc R U . . .
C16 C 0.2907(2) 0.8180(3) 0.77131(19) 0.0420(7) Uani 1 1 d . . . . .
H16 H 0.274519 0.901103 0.774303 0.050 Uiso 1 1 calc R U . . .
C5 C 0.1505(2) -0.0535(3) 0.93605(18) 0.0435(8) Uani 1 1 d . . . . .
C15 C 0.23882(19) 0.7321(3) 0.7227(2) 0.0439(8) Uani 1 1 d . . . . .
H15 H 0.187977 0.757823 0.692095 0.053 Uiso 1 1 calc R U . . .
C23 C 0.60752(18) 0.3879(4) 0.86715(18) 0.0483(9) Uani 1 1 d . . . . .
H23 H 0.652391 0.390689 0.852677 0.058 Uiso 1 1 calc R U . . .
C10 C 0.0216(2) 0.1956(3) 0.8486(2) 0.0534(9) Uani 1 1 d . . . . .
H10A H 0.024524 0.173950 0.900087 0.080 Uiso 1 1 calc R U . . .
H10B H -0.024232 0.248053 0.824836 0.080 Uiso 1 1 calc R U . . .
H10C H 0.068797 0.241101 0.850628 0.080 Uiso 1 1 calc R U . . .
C11 C 0.0006(2) 0.1103(4) 0.7170(2) 0.0570(10) Uani 1 1 d . . . . .
H11A H 0.043589 0.162346 0.714378 0.086 Uiso 1 1 calc R U . . .
H11B H -0.048563 0.156388 0.696443 0.086 Uiso 1 1 calc R U . . .
H11C H -0.002379 0.034378 0.687345 0.086 Uiso 1 1 calc R U . . .
C8 C 0.2193(2) -0.1441(4) 0.9457(2) 0.0636(11) Uani 1 1 d . . . . .
H8A H 0.199867 -0.219722 0.916099 0.095 Uiso 1 1 calc R U . . .
H8B H 0.243713 -0.165990 0.999339 0.095 Uiso 1 1 calc R U . . .
H8C H 0.257923 -0.103935 0.927871 0.095 Uiso 1 1 calc R U . . .
C7 C 0.1830(3) 0.0655(4) 0.9835(2) 0.0663(11) Uani 1 1 d . . . . .
H7A H 0.219050 0.107859 0.963272 0.099 Uiso 1 1 calc R U . . .
H7B H 0.210665 0.042157 1.036414 0.099 Uiso 1 1 calc R U . . .
H7C H 0.139757 0.121387 0.980858 0.099 Uiso 1 1 calc R U . . .
C12 C -0.0555(2) -0.0058(4) 0.8028(3) 0.0674(12) Uani 1 1 d . . . . .
H12A H -0.057231 -0.082875 0.774498 0.101 Uiso 1 1 calc R U . . .
H12B H -0.104073 0.040695 0.779489 0.101 Uiso 1 1 calc R U . . .
H12C H -0.049461 -0.025848 0.855366 0.101 Uiso 1 1 calc R U . . .
C31 C 0.1891(2) -0.0037(4) 0.5584(2) 0.0679(11) Uani 1 1 d . . . . .
H31A H 0.229198 0.039181 0.543936 0.102 Uiso 1 1 calc R U . . .
H31B H 0.195398 -0.093874 0.555140 0.102 Uiso 1 1 calc R U . . .
H31C H 0.194488 0.018856 0.610400 0.102 Uiso 1 1 calc R U . . .
C33 C 0.0416(2) -0.0202(4) 0.5249(2) 0.0669(11) Uani 1 1 d . . . . .
H33A H 0.049472 0.002202 0.578111 0.080 Uiso 1 1 calc R U . . .
H33B H 0.044828 -0.111985 0.522500 0.080 Uiso 1 1 calc R U . . .
C32 C 0.1078(2) 0.0349(5) 0.5044(2) 0.0685(11) Uani 1 1 d . . . . .
H32A H 0.103829 0.126806 0.504563 0.082 Uiso 1 1 calc R U . . .
H32B H 0.102237 0.008788 0.452290 0.082 Uiso 1 1 calc R U . . .
C6 C 0.0884(3) -0.1189(5) 0.9642(3) 0.0830(15) Uani 1 1 d . . . . .
H6A H 0.048044 -0.058804 0.964015 0.124 Uiso 1 1 calc R U . . .
H6B H 0.114067 -0.150400 1.015751 0.124 Uiso 1 1 calc R U . . .
H6C H 0.064504 -0.188353 0.930386 0.124 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
Fe1 P2 2.2246(7) . ?
Fe1 C4 1.841(3) . ?
Fe1 C3 1.781(3) . ?
Fe1 C2 1.781(3) . ?
Fe1 C1 1.788(3) . ?
P2 C19 1.834(3) . ?
P2 C25 1.830(2) . ?
P2 C13 1.822(3) . ?
P1 N1 1.714(2) . ?
P1 C9 1.874(3) . ?
P1 C5 1.870(3) . ?
O2 C2 1.146(3) . ?
O3 C3 1.150(3) . ?
O1 C1 1.146(3) . ?
N1 C4 1.158(3) . ?
C19 C20 1.390(4) . ?
C19 C24 1.379(4) . ?
C25 C30 1.391(4) . ?
C25 C26 1.386(4) . ?
C13 C14 1.397(4) . ?
C13 C18 1.381(4) . ?
C30 H30 0.9300 . ?
C30 C29 1.383(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.387(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.375(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.383(4) . ?
C24 H24 0.9300 . ?
C24 C23 1.382(4) . ?
C22 H22 0.9300 . ?
C22 C21 1.368(4) . ?
C22 C23 1.376(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.376(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.371(4) . ?
C28 C27 1.377(4) . ?
C9 C10 1.520(5) . ?
C9 C11 1.532(5) . ?
C9 C12 1.529(5) . ?
C21 H21 0.9300 . ?
C29 H29 0.9300 . ?
C27 H27 0.9300 . ?
C16 H16 0.9300 . ?
C16 C15 1.382(5) . ?
C5 C8 1.520(5) . ?
C5 C7 1.524(5) . ?
C5 C6 1.541(5) . ?
C15 H15 0.9300 . ?
C23 H23 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 C32 1.507(5) . ?
C33 C33 1.516(8) 3_556 ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C32 1.482(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
C4 Fe1 P2 177.25(9) . . ?
C3 Fe1 P2 92.90(9) . . ?
C3 Fe1 C4 89.22(12) . . ?
C3 Fe1 C1 115.03(13) . . ?
C2 Fe1 P2 87.69(9) . . ?
C2 Fe1 C4 89.70(12) . . ?
C2 Fe1 C3 122.29(13) . . ?
C2 Fe1 C1 122.68(13) . . ?
C1 Fe1 P2 90.22(9) . . ?
C1 Fe1 C4 90.47(12) . . ?
C19 P2 Fe1 113.55(8) . . ?
C25 P2 Fe1 117.08(9) . . ?
C25 P2 C19 103.37(11) . . ?
C13 P2 Fe1 114.39(8) . . ?
C13 P2 C19 103.40(12) . . ?
C13 P2 C25 103.44(12) . . ?
N1 P1 C9 97.98(13) . . ?
N1 P1 C5 97.89(14) . . ?
C5 P1 C9 112.77(15) . . ?
C4 N1 P1 174.5(2) . . ?
C20 C19 P2 118.75(19) . . ?
C24 C19 P2 122.7(2) . . ?
C24 C19 C20 118.6(2) . . ?
C30 C25 P2 119.5(2) . . ?
C26 C25 P2 121.4(2) . . ?
C26 C25 C30 119.1(2) . . ?
C14 C13 P2 118.2(2) . . ?
C18 C13 P2 122.8(2) . . ?
C18 C13 C14 118.9(3) . . ?
N1 C4 Fe1 179.9(3) . . ?
C25 C30 H30 119.9 . . ?
C29 C30 C25 120.2(3) . . ?
C29 C30 H30 119.9 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(3) . . ?
C21 C20 H20 119.6 . . ?
O3 C3 Fe1 176.3(3) . . ?
O2 C2 Fe1 178.5(3) . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.3(3) . . ?
C27 C26 H26 119.9 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C18 H18 119.8 . . ?
C13 C18 C17 120.3(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C24 H24 119.9 . . ?
C19 C24 C23 120.1(3) . . ?
C23 C24 H24 119.9 . . ?
C21 C22 H22 120.4 . . ?
C21 C22 C23 119.3(3) . . ?
C23 C22 H22 120.4 . . ?
O1 C1 Fe1 178.6(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 H17 119.8 . . ?
C29 C28 H28 119.9 . . ?
C29 C28 C27 120.2(3) . . ?
C27 C28 H28 119.9 . . ?
C10 C9 P1 116.7(2) . . ?
C10 C9 C11 109.3(3) . . ?
C10 C9 C12 111.0(3) . . ?
C11 C9 P1 104.4(2) . . ?
C12 C9 P1 107.4(2) . . ?
C12 C9 C11 107.6(3) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C30 C29 H29 119.9 . . ?
C28 C29 C30 120.3(3) . . ?
C28 C29 H29 119.9 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 119.9(3) . . ?
C28 C27 H27 120.0 . . ?
C17 C16 H16 120.0 . . ?
C17 C16 C15 119.9(3) . . ?
C15 C16 H16 120.0 . . ?
C8 C5 P1 104.3(2) . . ?
C8 C5 C7 108.4(3) . . ?
C8 C5 C6 109.2(3) . . ?
C7 C5 P1 116.1(2) . . ?
C7 C5 C6 110.5(3) . . ?
C6 C5 P1 107.9(3) . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.9(3) . . ?
C22 C23 H23 119.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
C33 C33 H33A 108.3 3_556 . ?
C33 C33 H33B 108.2 3_556 . ?
H33A C33 H33B 107.4 . . ?
C32 C33 C33 116.1(5) . 3_556 ?
C32 C33 H33A 108.3 . . ?
C32 C33 H33B 108.3 . . ?
C31 C32 H32A 108.8 . . ?
C31 C32 H32B 108.8 . . ?
C33 C32 C31 113.6(4) . . ?
C33 C32 H32A 108.8 . . ?
C33 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
Fe1 P2 C19 C20 -41.5(2) . . . . ?
Fe1 P2 C19 C24 138.3(2) . . . . ?
Fe1 P2 C25 C30 -31.5(2) . . . . ?
Fe1 P2 C25 C26 151.03(19) . . . . ?
Fe1 P2 C13 C14 -52.3(2) . . . . ?
Fe1 P2 C13 C18 125.0(2) . . . . ?
P2 C19 C20 C21 -179.6(2) . . . . ?
P2 C19 C24 C23 -179.8(3) . . . . ?
P2 C25 C30 C29 -176.8(2) . . . . ?
P2 C25 C26 C27 177.0(2) . . . . ?
P2 C13 C14 C15 177.0(2) . . . . ?
P2 C13 C18 C17 -175.9(2) . . . . ?
N1 P1 C9 C10 -57.6(3) . . . . ?
N1 P1 C9 C11 63.2(2) . . . . ?
N1 P1 C9 C12 177.2(3) . . . . ?
N1 P1 C5 C8 -79.7(3) . . . . ?
N1 P1 C5 C7 39.5(3) . . . . ?
N1 P1 C5 C6 164.2(3) . . . . ?
C19 P2 C25 C30 94.1(2) . . . . ?
C19 P2 C25 C26 -83.3(2) . . . . ?
C19 P2 C13 C14 -176.3(2) . . . . ?
C19 P2 C13 C18 1.0(2) . . . . ?
C19 C20 C21 C22 -0.8(5) . . . . ?
C19 C24 C23 C22 -0.4(5) . . . . ?
C25 P2 C19 C20 -169.4(2) . . . . ?
C25 P2 C19 C24 10.4(3) . . . . ?
C25 P2 C13 C14 76.2(2) . . . . ?
C25 P2 C13 C18 -106.5(2) . . . . ?
C25 C30 C29 C28 -0.6(4) . . . . ?
C25 C26 C27 C28 0.1(4) . . . . ?
C13 P2 C19 C20 83.0(2) . . . . ?
C13 P2 C19 C24 -97.2(3) . . . . ?
C13 P2 C25 C30 -158.3(2) . . . . ?
C13 P2 C25 C26 24.2(2) . . . . ?
C13 C14 C15 C16 -0.9(5) . . . . ?
C13 C18 C17 C16 -1.0(4) . . . . ?
C30 C25 C26 C27 -0.4(4) . . . . ?
C20 C19 C24 C23 0.0(5) . . . . ?
C26 C25 C30 C29 0.7(4) . . . . ?
C14 C13 C18 C17 1.3(4) . . . . ?
C18 C13 C14 C15 -0.4(4) . . . . ?
C18 C17 C16 C15 -0.4(5) . . . . ?
C24 C19 C20 C21 0.6(4) . . . . ?
C17 C16 C15 C14 1.3(5) . . . . ?
C9 P1 C5 C8 178.1(2) . . . . ?
C9 P1 C5 C7 -62.6(3) . . . . ?
C9 P1 C5 C6 62.0(3) . . . . ?
C21 C22 C23 C24 0.2(5) . . . . ?
C29 C28 C27 C26 -0.1(5) . . . . ?
C27 C28 C29 C30 0.3(5) . . . . ?
C5 P1 C9 C10 44.5(3) . . . . ?
C5 P1 C9 C11 165.2(2) . . . . ?
C5 P1 C9 C12 -80.8(3) . . . . ?
C23 C22 C21 C20 0.4(5) . . . . ?
C33 C33 C32 C31 177.1(5) 3_556 . . . ?


_ins_header                      
;
TITL RMK_376_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  17.900214  10.529076  18.428276  90.0000 110.2032  90.0000
ZERR    4.00   0.001739   0.000932   0.001894   0.0000   0.0115   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O P Fe
UNIT 132.00 160.00 4.00 12.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.905
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/hexane'
_chemical_properties_physical    Air-sensitive
