# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_1_gard25y
_database_code_depnum_ccdc_archive 'CCDC 2371547'
loop_
_audit_author_name
_audit_author_address
'James Gardinier'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_audit_creation_date             2024-03-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/1
loop_
_audit_author_email
james.gardinier@marquette.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H25 Br N4 O3 P Re'
_chemical_formula_sum            'C30 H25 Br N4 O3 P Re'
_chemical_formula_weight         786.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H25BrN4O3PRe
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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                   12.3314(2)
_cell_length_b                   13.5371(2)
_cell_length_c                   17.3610(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.9290(10)
_cell_angle_gamma                90
_cell_volume                     2824.62(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12870
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6110
_cell_measurement_theta_min      3.6430
_shelx_estimated_absorpt_T_max   0.354
_shelx_estimated_absorpt_T_min   0.127
_exptl_absorpt_coefficient_mu    10.932
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -5 -6 0.0813
4 5 6 0.0383
-7 3 6 0.1387
7 -3 -6 0.1387
6 1 -9 0.1000
-6 -1 9 0.1000
-7 1 -4 0.0906
7 -1 4 0.0906
2 7 -7 0.0962
0 -6 8 0.1269
-4 8 1 0.1438
4 -8 -1 0.1838

_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
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
-4.0032 -5.0066 -5.9927 0.9893 0.1736 0.0484
4.0032 5.0066 5.9927 -0.9893 -0.1736 -0.0484
-7.0012 3.0013 6.0063 0.0628 0.0003 -0.9984
7.0012 -3.0013 -6.0063 -0.0628 -0.0003 0.9984
5.9990 0.9976 -9.0085 -0.1449 0.5288 0.8332
-5.9990 -0.9976 9.0085 0.1449 -0.5288 -0.8332
-7.0047 0.9950 -3.9935 0.6839 0.5556 -0.5656
7.0047 -0.9950 3.9935 -0.6839 -0.5556 0.5656
1.9970 6.9987 -7.0082 -0.3685 0.9398 0.1249
0.0041 -5.9970 8.0054 0.0818 -0.9953 -0.0145
-4.0027 8.0011 0.9987 -0.3290 0.6260 -0.7610
4.0027 -8.0011 -0.9987 0.3290 -0.6260 0.7610

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        70.648
_diffrn_reflns_theta_max         70.648
_diffrn_reflns_theta_min         4.007
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_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   -117.00 -18.00   1.00    1.00    --  -42.46 -37.00  30.00   99
  2  ω    -81.00  27.00   1.00    1.00    --  -42.46  93.00 -67.00  108
  3  ω     23.00  98.00   1.00    1.00    --   42.46-125.00-150.00   75
  4  ω    101.00 178.00   1.00    1.12    --  100.00  93.00 -67.00   77
  5  ω     27.00 118.00   1.00    1.12    --  100.00-125.00 120.00   91
  6  ω     27.00 118.00   1.00    1.12    --  100.00-125.00  30.00   91
  7  ω     27.00 118.00   1.00    1.12    --  100.00-125.00-120.00   91
  8  ω     74.00 173.00   1.00    1.12    --  100.00  45.00   0.00   99
  9  ω     47.00 178.00   1.00    1.12    --  100.00  15.00 120.00  131
 10  ω     94.00 173.00   1.00    1.12    --  100.00 125.00 150.00   79
 11  ω   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00 -30.00  109
 12  ω   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00-120.00  101
 13  ω   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00 150.00  101
 14  ω     94.00 140.00   1.00    1.12    --  100.00 125.00  30.00   46
 15  ω     71.00 172.00   1.00    1.12    --  100.00  61.00-180.00  101
 16  ω     72.00 176.00   1.00    1.12    --  100.00  30.00 -90.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0817770000
_diffrn_orient_matrix_UB_12      -0.0761836000
_diffrn_orient_matrix_UB_13      -0.0468062000
_diffrn_orient_matrix_UB_21      -0.0290889000
_diffrn_orient_matrix_UB_22      0.0724356000
_diffrn_orient_matrix_UB_23      -0.0700478000
_diffrn_orient_matrix_UB_31      0.0942451000
_diffrn_orient_matrix_UB_32      -0.0436512000
_diffrn_orient_matrix_UB_33      -0.0345635000
_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                4982
_reflns_number_total             5354
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.138
_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)+(0.0340P)²+4.0831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_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. Others
 Fixed Sof: Br1A(0.8) Br1B(0.2) O2A(0.8) O2B(0.2) C9A(0.8) C9B(0.2)
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_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 0.59843(2) 0.47283(2) 0.34669(2) 0.01755(7) Uani 1 1 d . . . . .
Br1A Br 0.49653(6) 0.63429(7) 0.37173(4) 0.01993(15) Uani 0.8 1 d . . P A 1
Br1B Br 0.6772(3) 0.3002(4) 0.3465(3) 0.0277(10) Uani 0.2 1 d . . P A -1
P1 P 0.54117(8) 0.48965(7) 0.20043(6) 0.0161(2) Uani 1 1 d . . . . .
O3 O 0.6943(3) 0.4637(2) 0.52756(19) 0.0346(8) Uani 1 1 d . . . . .
O1 O 0.8164(3) 0.5755(3) 0.3358(2) 0.0376(8) Uani 1 1 d . . . . .
O2A O 0.6963(7) 0.2650(6) 0.3365(5) 0.036(2) Uani 0.8 1 d . . P A 1
O2B O 0.4815(18) 0.6657(15) 0.3733(12) 0.018(6) Uiso 0.2 1 d . . P A -1
N11 N 0.3372(3) 0.4103(2) 0.31819(19) 0.0190(7) Uani 1 1 d . . . . .
N12 N 0.4448(3) 0.3962(2) 0.35839(19) 0.0177(7) Uani 1 1 d . . . . .
N21 N 0.2093(3) 0.5246(2) 0.2414(2) 0.0199(7) Uani 1 1 d . . . . .
N22 N 0.1084(3) 0.4779(3) 0.2262(3) 0.0303(9) Uani 1 1 d . . . . .
C1 C 0.4240(3) 0.4119(3) 0.1501(2) 0.0185(8) Uani 1 1 d . . . . .
C2 C 0.3231(3) 0.4106(3) 0.1757(2) 0.0169(8) Uani 1 1 d . . . . .
C3 C 0.2380(3) 0.3478(3) 0.1390(2) 0.0205(8) Uani 1 1 d . . . . .
H3 H 0.171756 0.346468 0.156056 0.025 Uiso 1 1 calc R U . . .
C4 C 0.2507(3) 0.2872(3) 0.0773(3) 0.0247(9) Uani 1 1 d . . . . .
H4 H 0.193161 0.245241 0.053553 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3487(3) 0.2889(3) 0.0508(2) 0.0252(9) Uani 1 1 d . . . . .
H5 H 0.357060 0.248342 0.009303 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4343(3) 0.3515(3) 0.0868(2) 0.0215(8) Uani 1 1 d . . . . .
H6 H 0.499585 0.353366 0.068508 0.026 Uiso 1 1 calc R U . . .
C7 C 0.3128(3) 0.4725(3) 0.2465(2) 0.0179(8) Uani 1 1 d . . . . .
H7 H 0.371525 0.522678 0.253276 0.021 Uiso 1 1 calc R U . . .
C10 C 0.6547(4) 0.4666(3) 0.4625(3) 0.0232(9) Uani 1 1 d . . . . .
C8 C 0.7344(4) 0.5380(3) 0.3393(2) 0.0244(9) Uani 1 1 d . . . . .
C9A C 0.6604(7) 0.3458(6) 0.3361(5) 0.0257(19) Uani 0.8 1 d . . P A 1
C9B C 0.527(2) 0.601(2) 0.3684(16) 0.025(8) Uiso 0.2 1 d . . P A -1
C11 C 0.2677(3) 0.3496(3) 0.3446(3) 0.0253(9) Uani 1 1 d . . . . .
H11 H 0.191277 0.344669 0.325086 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3306(4) 0.2959(4) 0.4060(3) 0.0298(10) Uani 1 1 d . . . . .
H12 H 0.305632 0.248695 0.436928 0.036 Uiso 1 1 calc R U . . .
C13 C 0.4386(4) 0.3271(3) 0.4117(3) 0.0260(9) Uani 1 1 d . . . . .
H13 H 0.499588 0.302829 0.448316 0.031 Uiso 1 1 calc R U . . .
C21 C 0.1999(4) 0.6211(3) 0.2590(3) 0.0316(10) Uani 1 1 d . . . . .
H21 H 0.257622 0.666534 0.271986 0.038 Uiso 1 1 calc R U . . .
C22 C 0.0902(4) 0.6390(4) 0.2544(3) 0.0388(12) Uani 1 1 d . . . . .
H22 H 0.057411 0.698652 0.263003 0.047 Uiso 1 1 calc R U . . .
C23 C 0.0377(4) 0.5492(4) 0.2339(3) 0.0303(10) Uani 1 1 d . . . . .
H23 H -0.038689 0.539832 0.226478 0.036 Uiso 1 1 calc R U . . .
C31 C 0.6545(3) 0.4604(3) 0.1511(2) 0.0184(8) Uani 1 1 d . . . . .
C32 C 0.6979(3) 0.5316(3) 0.1087(3) 0.0227(9) Uani 1 1 d . . . . .
H32 H 0.666721 0.594504 0.103214 0.027 Uiso 1 1 calc R U . . .
C33 C 0.7860(3) 0.5111(3) 0.0745(3) 0.0231(9) Uani 1 1 d . . . . .
H33 H 0.813072 0.560167 0.046338 0.028 Uiso 1 1 calc R U . . .
C34 C 0.8353(3) 0.4173(3) 0.0817(2) 0.0196(8) Uani 1 1 d . . . . .
C35 C 0.7918(3) 0.3466(3) 0.1241(2) 0.0211(8) Uani 1 1 d . . . . .
H35 H 0.822770 0.283632 0.129362 0.025 Uiso 1 1 calc R U . . .
C36 C 0.7039(3) 0.3669(3) 0.1588(2) 0.0218(9) Uani 1 1 d . . . . .
H36 H 0.677396 0.318004 0.187415 0.026 Uiso 1 1 calc R U . . .
C37 C 0.9320(3) 0.3970(3) 0.0450(3) 0.0246(9) Uani 1 1 d . . . . .
H37A H 0.994418 0.436446 0.070580 0.037 Uiso 1 1 calc R U . . .
H37B H 0.912221 0.413064 -0.010184 0.037 Uiso 1 1 calc R U . . .
H37C H 0.951467 0.328283 0.051239 0.037 Uiso 1 1 calc R U . . .
C41 C 0.5019(3) 0.6134(3) 0.1617(2) 0.0176(8) Uani 1 1 d . . . . .
C42 C 0.4278(3) 0.6276(3) 0.0895(2) 0.0195(8) Uani 1 1 d . . . . .
H42 H 0.388004 0.574285 0.063553 0.023 Uiso 1 1 calc R U . . .
C43 C 0.4130(3) 0.7209(3) 0.0561(2) 0.0213(8) Uani 1 1 d . . . . .
H43 H 0.363426 0.729240 0.007665 0.026 Uiso 1 1 calc R U . . .
C44 C 0.4710(3) 0.8028(3) 0.0935(2) 0.0217(8) Uani 1 1 d . . . . .
C45 C 0.5430(3) 0.7878(3) 0.1666(2) 0.0219(8) Uani 1 1 d . . . . .
H45 H 0.581055 0.841416 0.193345 0.026 Uiso 1 1 calc R U . . .
C46 C 0.5590(3) 0.6951(3) 0.2002(2) 0.0206(8) Uani 1 1 d . . . . .
H46 H 0.608120 0.686922 0.248922 0.025 Uiso 1 1 calc R U . . .
C47 C 0.4578(4) 0.9035(3) 0.0563(3) 0.0315(10) Uani 1 1 d . . . . .
H47A H 0.409620 0.942747 0.080351 0.047 Uiso 1 1 calc R U . . .
H47B H 0.426119 0.897226 0.000733 0.047 Uiso 1 1 calc R U . . .
H47C H 0.529288 0.934768 0.063988 0.047 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Br1A 2.6057(11) . ?
Re1 Br1B 2.531(5) . ?
Re1 P1 2.4892(10) . ?
Re1 N12 2.209(3) . ?
Re1 C10 1.976(4) . ?
Re1 C8 1.925(4) . ?
Re1 C9A 1.907(9) . ?
Re1 C9B 2.02(3) . ?
Br1A C9B 0.60(3) . ?
Br1B O2A 0.575(5) . ?
Br1B C9A 0.664(6) . ?
P1 C1 1.842(4) . ?
P1 C31 1.837(4) . ?
P1 C41 1.830(4) . ?
O3 C10 1.127(5) . ?
O1 C8 1.145(5) . ?
O2A C9A 1.179(10) . ?
O2B C9B 1.06(3) . ?
N11 N12 1.367(4) . ?
N11 C7 1.477(5) . ?
N11 C11 1.340(5) . ?
N12 C13 1.329(5) . ?
N21 N22 1.367(5) . ?
N21 C7 1.444(5) . ?
N21 C21 1.352(5) . ?
N22 C23 1.327(6) . ?
C1 C2 1.411(5) . ?
C1 C6 1.398(6) . ?
C2 C3 1.389(5) . ?
C2 C7 1.516(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.386(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.377(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(6) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.359(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.386(7) . ?
C23 H23 0.9300 . ?
C31 C32 1.392(6) . ?
C31 C36 1.399(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.377(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.401(6) . ?
C34 C35 1.387(6) . ?
C34 C37 1.498(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.379(6) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.389(5) . ?
C41 C46 1.399(5) . ?
C42 H42 0.9300 . ?
C42 C43 1.384(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.398(6) . ?
C44 C45 1.391(6) . ?
C44 C47 1.502(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.379(6) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 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
Br1B Re1 Br1A 166.97(11) . . ?
P1 Re1 Br1A 93.22(3) . . ?
P1 Re1 Br1B 96.00(11) . . ?
N12 Re1 Br1A 85.60(9) . . ?
N12 Re1 Br1B 84.48(13) . . ?
N12 Re1 P1 94.78(9) . . ?
C10 Re1 Br1A 86.50(12) . . ?
C10 Re1 Br1B 85.08(16) . . ?
C10 Re1 P1 175.18(12) . . ?
C10 Re1 N12 90.00(15) . . ?
C10 Re1 C9B 85.1(8) . . ?
C8 Re1 Br1A 94.95(13) . . ?
C8 Re1 Br1B 94.75(16) . . ?
C8 Re1 P1 86.72(12) . . ?
C8 Re1 N12 178.37(15) . . ?
C8 Re1 C10 88.50(17) . . ?
C8 Re1 C9B 92.4(8) . . ?
C9A Re1 Br1A 172.3(2) . . ?
C9A Re1 Br1B 5.9(3) . . ?
C9A Re1 P1 90.7(2) . . ?
C9A Re1 N12 87.5(3) . . ?
C9A Re1 C10 90.2(3) . . ?
C9A Re1 C8 91.9(3) . . ?
C9A Re1 C9B 173.5(8) . . ?
C9B Re1 Br1A 2.8(8) . . ?
C9B Re1 Br1B 167.7(8) . . ?
C9B Re1 P1 94.4(8) . . ?
C9B Re1 N12 88.1(8) . . ?
C9B Br1A Re1 10(3) . . ?
O2A Br1B Re1 161.5(14) . . ?
O2A Br1B C9A 144.3(19) . . ?
C9A Br1B Re1 17.2(9) . . ?
C1 P1 Re1 116.41(13) . . ?
C31 P1 Re1 112.56(13) . . ?
C31 P1 C1 104.71(18) . . ?
C41 P1 Re1 116.74(13) . . ?
C41 P1 C1 103.51(18) . . ?
C41 P1 C31 101.10(18) . . ?
Br1B O2A C9A 19.2(11) . . ?
N12 N11 C7 120.1(3) . . ?
C11 N11 N12 111.2(3) . . ?
C11 N11 C7 127.8(3) . . ?
N11 N12 Re1 129.9(2) . . ?
C13 N12 Re1 125.3(3) . . ?
C13 N12 N11 104.7(3) . . ?
N22 N21 C7 122.7(3) . . ?
C21 N21 N22 111.7(3) . . ?
C21 N21 C7 125.3(4) . . ?
C23 N22 N21 103.6(4) . . ?
C2 C1 P1 120.8(3) . . ?
C6 C1 P1 120.4(3) . . ?
C6 C1 C2 118.8(4) . . ?
C1 C2 C7 119.1(3) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 C7 121.2(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.3(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.5(4) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 H6 119.4 . . ?
N11 C7 C2 109.3(3) . . ?
N11 C7 H7 106.7 . . ?
N21 C7 N11 109.9(3) . . ?
N21 C7 C2 117.0(3) . . ?
N21 C7 H7 106.7 . . ?
C2 C7 H7 106.7 . . ?
O3 C10 Re1 175.1(4) . . ?
O1 C8 Re1 178.7(4) . . ?
Br1B C9A Re1 156.9(12) . . ?
Br1B C9A O2A 16.5(9) . . ?
O2A C9A Re1 173.4(8) . . ?
Br1A C9B Re1 168(3) . . ?
Br1A C9B O2B 7.2(14) . . ?
O2B C9B Re1 173(3) . . ?
N11 C11 H11 126.4 . . ?
N11 C11 C12 107.2(4) . . ?
C12 C11 H11 126.4 . . ?
C11 C12 H12 127.4 . . ?
C11 C12 C13 105.1(4) . . ?
C13 C12 H12 127.4 . . ?
N12 C13 C12 111.8(4) . . ?
N12 C13 H13 124.1 . . ?
C12 C13 H13 124.1 . . ?
N21 C21 H21 126.5 . . ?
N21 C21 C22 107.1(4) . . ?
C22 C21 H21 126.5 . . ?
C21 C22 H22 127.5 . . ?
C21 C22 C23 105.1(4) . . ?
C23 C22 H22 127.5 . . ?
N22 C23 C22 112.5(4) . . ?
N22 C23 H23 123.7 . . ?
C22 C23 H23 123.7 . . ?
C32 C31 P1 121.4(3) . . ?
C32 C31 C36 117.8(4) . . ?
C36 C31 P1 120.8(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.5(4) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.9(4) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C37 120.0(4) . . ?
C35 C34 C33 117.5(4) . . ?
C35 C34 C37 122.5(4) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 C34 121.9(4) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.5(4) . . ?
C35 C36 H36 119.8 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 P1 121.6(3) . . ?
C42 C41 C46 118.8(4) . . ?
C46 C41 P1 119.0(3) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 120.1(4) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 119.2 . . ?
C42 C43 C44 121.6(4) . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C47 121.7(4) . . ?
C45 C44 C43 117.6(4) . . ?
C45 C44 C47 120.7(4) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 C44 121.3(4) . . ?
C46 C45 H45 119.3 . . ?
C41 C46 H46 119.7 . . ?
C45 C46 C41 120.5(4) . . ?
C45 C46 H46 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 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 Br1A C9B O2B 148(15) . . . . ?
Re1 Br1B O2A C9A 1(2) . . . . ?
Re1 Br1B C9A O2A -179(3) . . . . ?
Re1 P1 C1 C2 51.4(4) . . . . ?
Re1 P1 C1 C6 -127.3(3) . . . . ?
Re1 P1 C31 C32 -116.3(3) . . . . ?
Re1 P1 C31 C36 60.2(3) . . . . ?
Re1 P1 C41 C42 -152.8(3) . . . . ?
Re1 P1 C41 C46 36.1(4) . . . . ?
Re1 N12 C13 C12 177.8(3) . . . . ?
P1 C1 C2 C3 -177.0(3) . . . . ?
P1 C1 C2 C7 -1.3(5) . . . . ?
P1 C1 C6 C5 176.8(3) . . . . ?
P1 C31 C32 C33 177.2(3) . . . . ?
P1 C31 C36 C35 -177.5(3) . . . . ?
P1 C41 C42 C43 -169.9(3) . . . . ?
P1 C41 C46 C45 170.6(3) . . . . ?
O2A Br1B C9A Re1 179(3) . . . . ?
N11 N12 C13 C12 0.8(5) . . . . ?
N11 C11 C12 C13 -1.5(5) . . . . ?
N12 N11 C7 N21 -145.8(3) . . . . ?
N12 N11 C7 C2 84.6(4) . . . . ?
N12 N11 C11 C12 2.1(5) . . . . ?
N21 N22 C23 C22 -0.7(6) . . . . ?
N21 C21 C22 C23 0.4(6) . . . . ?
N22 N21 C7 N11 -69.3(5) . . . . ?
N22 N21 C7 C2 56.0(5) . . . . ?
N22 N21 C21 C22 -0.9(6) . . . . ?
C1 P1 C31 C32 116.3(3) . . . . ?
C1 P1 C31 C36 -67.1(4) . . . . ?
C1 P1 C41 C42 -23.5(4) . . . . ?
C1 P1 C41 C46 165.4(3) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C7 N11 -95.8(4) . . . . ?
C1 C2 C7 N21 138.5(4) . . . . ?
C2 C1 C6 C5 -2.0(6) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C3 C2 C7 N11 79.8(4) . . . . ?
C3 C2 C7 N21 -45.8(5) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
C4 C5 C6 C1 1.0(6) . . . . ?
C6 C1 C2 C3 1.7(6) . . . . ?
C6 C1 C2 C7 177.4(3) . . . . ?
C7 N11 N12 Re1 11.8(5) . . . . ?
C7 N11 N12 C13 -171.5(3) . . . . ?
C7 N11 C11 C12 170.8(4) . . . . ?
C7 N21 N22 C23 174.3(4) . . . . ?
C7 N21 C21 C22 -174.0(4) . . . . ?
C7 C2 C3 C4 -176.2(4) . . . . ?
C11 N11 N12 Re1 -178.5(3) . . . . ?
C11 N11 N12 C13 -1.8(4) . . . . ?
C11 N11 C7 N21 46.4(5) . . . . ?
C11 N11 C7 C2 -83.2(5) . . . . ?
C11 C12 C13 N12 0.4(5) . . . . ?
C21 N21 N22 C23 0.9(5) . . . . ?
C21 N21 C7 N11 103.1(5) . . . . ?
C21 N21 C7 C2 -131.6(4) . . . . ?
C21 C22 C23 N22 0.2(6) . . . . ?
C31 P1 C1 C2 176.4(3) . . . . ?
C31 P1 C1 C6 -2.3(4) . . . . ?
C31 P1 C41 C42 84.8(3) . . . . ?
C31 P1 C41 C46 -86.4(3) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C32 C31 C36 C35 -0.8(6) . . . . ?
C32 C33 C34 C35 0.1(6) . . . . ?
C32 C33 C34 C37 -179.2(4) . . . . ?
C33 C34 C35 C36 -0.5(6) . . . . ?
C34 C35 C36 C31 0.8(6) . . . . ?
C36 C31 C32 C33 0.5(6) . . . . ?
C37 C34 C35 C36 178.8(4) . . . . ?
C41 P1 C1 C2 -78.1(3) . . . . ?
C41 P1 C1 C6 103.2(3) . . . . ?
C41 P1 C31 C32 9.0(4) . . . . ?
C41 P1 C31 C36 -174.5(3) . . . . ?
C41 C42 C43 C44 -0.3(6) . . . . ?
C42 C41 C46 C45 -0.8(6) . . . . ?
C42 C43 C44 C45 -1.2(6) . . . . ?
C42 C43 C44 C47 178.1(4) . . . . ?
C43 C44 C45 C46 1.6(6) . . . . ?
C44 C45 C46 C41 -0.7(6) . . . . ?
C46 C41 C42 C43 1.3(6) . . . . ?
C47 C44 C45 C46 -177.6(4) . . . . ?

_olex2_submission_original_sample_id gard25y
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.634
####################################################################### 
# 
# 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_3-Mn_gard25n
_database_code_depnum_ccdc_archive 'CCDC 2371552'
loop_
_audit_author_name
_audit_author_address
'Alexander N Erickson'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-08-27 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30.84 H27.51 Mn N4.84 O2.16 P, C F3 O3 S'
_chemical_formula_sum            'C31.84 H27.51 F3 Mn N4.84 O5.16 P S'
_chemical_formula_weight         735.42

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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   16.4795(2)
_cell_length_b                   12.8391(2)
_cell_length_c                   16.5133(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.4813(18)
_cell_angle_gamma                90
_cell_volume                     3251.19(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    12814
_cell_measurement_theta_min      4.4570
_cell_measurement_theta_max      70.5240

_exptl_crystal_description       Plate
_exptl_crystal_colour            'Clear Yellow'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_F_000             1507
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.028
_exptl_absorpt_coefficient_mu    4.950
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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   ?
_diffrn_ambient_temperature      100.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Supernova (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_source_current           0.80
_diffrn_measurement_device_type  'Oxford Diffraction Supernova, Dual Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support 'MiTeGen Dual Thickness MicroMount'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryojet Controller'
_diffrn_detector                 'CCD Plate'
_diffrn_detector_type            'Oxford Diffraction Atlas, 135 mm'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_reflns_number            30350
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.488
_diffrn_reflns_theta_max         70.541
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6176
_reflns_number_gt                5708
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_refine_special_details          
;
The initial refinement of the structure determined there was additional electron 
density around the CH3CN molecule (N1 C15 C16), this was initially ignored as it 
was less than 10% contribution. After further consideration, we have decided to 
model this additional density as partially occupied CO. The occupancies of both 
the CO and CH3CN were constrained to a sum of 1 and refined to 0.835(7) for the 
major component (N1 C15 C16) and 0.165(7) for the minor component (C10 O10). 
C10 of the CO molecule and N1 of the CH3CN had their coordinates constrained 
with EXYZ. Additionally, C10 of the CO molecule and N1 of the CH3CN had their 
displacement parameters constrained with EADP.  

Further investigation has determined that the triflate molecule 
(C14 F1 F2 F3 S3 O3 O4 O5) is most likely disorderred across two sites. 
The careful inspection has revealed the highest Q peak is 0.5 electrons. 
Modeling such disorder would rrequire heavy restraints due to the low 
density available. Therefore we have decided not to model this disorder 
because no other valuable information would be gained by doing so.

All hydrogen atoms were placed in calculated positions and had their thermal 
parameters tied to the isotropic thermal parameters of the atoms to which they 
were bonded (1.5x for methyl, 1.2x for others).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²+2.3653P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6176
_refine_ls_number_parameters     446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.51413(2) 0.27364(2) 0.29751(2) 0.01703(9) Uani 1 1 d . . . . .
P1 P 0.40304(3) 0.38821(4) 0.28071(3) 0.01640(11) Uani 1 1 d . . . . .
O1 O 0.49069(10) 0.16321(13) 0.44330(9) 0.0291(3) Uani 1 1 d . . . . .
O2 O 0.63554(9) 0.40809(13) 0.43310(10) 0.0299(3) Uani 1 1 d . . . . .
N11 N 0.39145(10) 0.18937(13) 0.12339(10) 0.0186(3) Uani 1 1 d . . . . .
N12 N 0.42547(10) 0.17546(13) 0.21076(10) 0.0190(3) Uani 1 1 d . . . . .
N21 N 0.47963(10) 0.33285(13) 0.11010(10) 0.0189(3) Uani 1 1 d . . . . .
N22 N 0.53442(10) 0.34018(13) 0.19431(10) 0.0194(3) Uani 1 1 d . . . . .
C10 C 0.60547(11) 0.17512(15) 0.29339(12) 0.0247(4) Uani 0.164(8) 1 d . . P A 1
O10 O 0.6541(14) 0.1135(17) 0.3062(12) 0.030(4) Uani 0.164(8) 1 d . . P A 1
N1 N 0.60547(11) 0.17512(15) 0.29339(12) 0.0247(4) Uani 0.836(8) 1 d . . P A 2
C15 C 0.6565(4) 0.1269(5) 0.2769(3) 0.0273(10) Uani 0.836(8) 1 d . . P A 2
C16 C 0.72120(19) 0.0653(3) 0.2570(2) 0.0446(10) Uani 0.836(8) 1 d . . P A 2
H16A H 0.778572 0.090050 0.291009 0.067 Uiso 0.836(8) 1 calc R U P A 2
H16B H 0.711558 0.071703 0.196260 0.067 Uiso 0.836(8) 1 calc R U P A 2
H16C H 0.716086 -0.006534 0.270679 0.067 Uiso 0.836(8) 1 calc R U P A 2
C9 C 0.49858(13) 0.20773(16) 0.38602(13) 0.0215(4) Uani 1 1 d . . . . .
C8 C 0.59005(13) 0.35692(17) 0.37793(13) 0.0226(4) Uani 1 1 d . . . . .
C11 C 0.34203(13) 0.10689(16) 0.08263(14) 0.0224(4) Uani 1 1 d . . . . .
H11 H 0.311485 0.099925 0.023118 0.027 Uiso 1 1 calc R U . . .
C12 C 0.34553(13) 0.03589(17) 0.14547(14) 0.0246(4) Uani 1 1 d . . . . .
H12 H 0.318565 -0.028934 0.137708 0.029 Uiso 1 1 calc R U . . .
C13 C 0.39815(13) 0.08144(16) 0.22367(13) 0.0229(4) Uani 1 1 d . . . . .
H13 H 0.412388 0.050211 0.277935 0.027 Uiso 1 1 calc R U . . .
C21 C 0.51481(13) 0.37766(16) 0.05623(13) 0.0233(4) Uani 1 1 d . . . . .
H21 H 0.489118 0.382539 -0.004033 0.028 Uiso 1 1 calc R U . . .
C22 C 0.59515(13) 0.41429(17) 0.10716(14) 0.0249(4) Uani 1 1 d . . . . .
H22 H 0.634754 0.449372 0.088843 0.030 Uiso 1 1 calc R U . . .
C23 C 0.60540(13) 0.38824(16) 0.19207(14) 0.0229(4) Uani 1 1 d . . . . .
H23 H 0.654976 0.402377 0.240709 0.027 Uiso 1 1 calc R U . . .
C1 C 0.32152(12) 0.40857(15) 0.16976(12) 0.0183(4) Uani 1 1 d . . . . .
C2 C 0.32400(12) 0.36510(15) 0.09230(13) 0.0192(4) Uani 1 1 d . . . . .
C3 C 0.25732(14) 0.38899(17) 0.01297(14) 0.0260(4) Uani 1 1 d . . . . .
H3 H 0.258287 0.359266 -0.038032 0.031 Uiso 1 1 calc R U . . .
C4 C 0.18999(14) 0.45592(18) 0.00887(14) 0.0284(5) Uani 1 1 d . . . . .
H4 H 0.146486 0.471070 -0.044458 0.034 Uiso 1 1 calc R U . . .
C5 C 0.18772(13) 0.50006(17) 0.08424(14) 0.0257(4) Uani 1 1 d . . . . .
H5 H 0.142885 0.545310 0.082021 0.031 Uiso 1 1 calc R U . . .
C6 C 0.25294(13) 0.47630(16) 0.16340(13) 0.0224(4) Uani 1 1 d . . . . .
H6 H 0.250982 0.506415 0.213873 0.027 Uiso 1 1 calc R U . . .
C7 C 0.39173(12) 0.29038(15) 0.08345(12) 0.0188(4) Uani 1 1 d . . . . .
H7 H 0.373880 0.276646 0.020948 0.023 Uiso 1 1 calc R U . . .
C41 C 0.33584(12) 0.34780(15) 0.34143(13) 0.0188(4) Uani 1 1 d . . . . .
C42 C 0.36562(13) 0.36320(17) 0.43128(13) 0.0230(4) Uani 1 1 d . . . . .
H42 H 0.416533 0.400870 0.458748 0.028 Uiso 1 1 calc R U . . .
C43 C 0.32001(13) 0.32286(17) 0.47994(14) 0.0252(4) Uani 1 1 d . . . . .
H43 H 0.339818 0.335609 0.539473 0.030 Uiso 1 1 calc R U . . .
C44 C 0.24491(14) 0.26349(17) 0.44101(14) 0.0256(4) Uani 1 1 d . . . . .
C45 C 0.21593(13) 0.24728(17) 0.35172(14) 0.0251(4) Uani 1 1 d . . . . .
H45 H 0.165833 0.208079 0.324557 0.030 Uiso 1 1 calc R U . . .
C46 C 0.26073(13) 0.28881(16) 0.30228(13) 0.0211(4) Uani 1 1 d . . . . .
H46 H 0.240304 0.277053 0.242579 0.025 Uiso 1 1 calc R U . . .
C47 C 0.19749(17) 0.2172(2) 0.49484(17) 0.0384(6) Uani 1 1 d . . . . .
H47A H 0.239045 0.190505 0.548214 0.058 Uiso 1 1 calc R U . . .
H47B H 0.160489 0.161691 0.463035 0.058 Uiso 1 1 calc R U . . .
H47C H 0.162654 0.269992 0.507623 0.058 Uiso 1 1 calc R U . . .
C31 C 0.43276(12) 0.52406(16) 0.31150(12) 0.0198(4) Uani 1 1 d . . . . .
C36 C 0.49369(13) 0.56941(16) 0.28217(13) 0.0220(4) Uani 1 1 d . . . . .
H36 H 0.519232 0.529384 0.250997 0.026 Uiso 1 1 calc R U . . .
C35 C 0.51689(13) 0.67317(17) 0.29864(13) 0.0237(4) Uani 1 1 d . . . . .
H35 H 0.557505 0.701817 0.278082 0.028 Uiso 1 1 calc R U . . .
C34 C 0.48035(14) 0.73518(16) 0.34549(13) 0.0232(4) Uani 1 1 d . . . . .
C33 C 0.41996(13) 0.68992(16) 0.37557(13) 0.0222(4) Uani 1 1 d . . . . .
H33 H 0.395381 0.729884 0.407642 0.027 Uiso 1 1 calc R U . . .
C32 C 0.39564(12) 0.58593(16) 0.35857(13) 0.0214(4) Uani 1 1 d . . . . .
H32 H 0.354551 0.557495 0.378587 0.026 Uiso 1 1 calc R U . . .
C37 C 0.50691(16) 0.84765(17) 0.36311(15) 0.0314(5) Uani 1 1 d . . . . .
H37A H 0.462549 0.885236 0.375693 0.047 Uiso 1 1 calc R U . . .
H37B H 0.514170 0.877362 0.312844 0.047 Uiso 1 1 calc R U . . .
H37C H 0.560932 0.852057 0.412029 0.047 Uiso 1 1 calc R U . . .
S3 S 0.85500(3) 0.30580(5) 0.34291(3) 0.02759(13) Uani 1 1 d . . . . .
F1 F 0.98724(10) 0.37155(13) 0.47732(9) 0.0469(4) Uani 1 1 d . . . . .
F2 F 1.01886(10) 0.33902(15) 0.36462(11) 0.0519(4) Uani 1 1 d . . . . .
F3 F 0.94914(11) 0.47709(13) 0.36955(12) 0.0569(4) Uani 1 1 d . . . . .
O3 O 0.88057(12) 0.20236(15) 0.37561(12) 0.0472(5) Uani 1 1 d . . . . .
O4 O 0.83198(10) 0.31797(14) 0.25074(10) 0.0325(4) Uani 1 1 d . . . . .
O5 O 0.79778(11) 0.35733(18) 0.37786(11) 0.0491(5) Uani 1 1 d . . . . .
C14 C 0.95775(16) 0.3779(2) 0.39089(16) 0.0362(5) 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
Mn1 C9 1.787(2) . ?
Mn1 C8 1.804(2) . ?
Mn1 N1 1.9863(19) . ?
Mn1 C10 1.9863(19) . ?
Mn1 N22 2.0403(17) . ?
Mn1 N12 2.0597(16) . ?
Mn1 P1 2.2848(5) . ?
P1 C41 1.8205(19) . ?
P1 C31 1.833(2) . ?
P1 C1 1.8512(19) . ?
O1 C9 1.153(3) . ?
O2 C8 1.150(3) . ?
N11 N12 1.355(2) . ?
N11 C11 1.355(3) . ?
N11 C7 1.456(3) . ?
N12 C13 1.333(3) . ?
N21 C21 1.355(3) . ?
N21 N22 1.356(2) . ?
N21 C7 1.457(2) . ?
N22 C23 1.335(3) . ?
C10 O10 1.09(2) . ?
N1 C15 1.154(7) . ?
C15 C16 1.459(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C11 C12 1.366(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.393(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C21 C22 1.366(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.390(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C1 C6 1.399(3) . ?
C1 C2 1.410(3) . ?
C2 C3 1.401(3) . ?
C2 C7 1.519(3) . ?
C3 C4 1.385(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C41 C46 1.392(3) . ?
C41 C42 1.396(3) . ?
C42 C43 1.386(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.394(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.389(3) . ?
C44 C47 1.504(3) . ?
C45 C46 1.392(3) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C31 C36 1.392(3) . ?
C31 C32 1.399(3) . ?
C36 C35 1.385(3) . ?
C36 H36 0.9300 . ?
C35 C34 1.391(3) . ?
C35 H35 0.9300 . ?
C34 C33 1.392(3) . ?
C34 C37 1.506(3) . ?
C33 C32 1.393(3) . ?
C33 H33 0.9300 . ?
C32 H32 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
S3 O5 1.4348(18) . ?
S3 O4 1.4360(16) . ?
S3 O3 1.4374(19) . ?
S3 C14 1.835(3) . ?
F1 C14 1.331(3) . ?
F2 C14 1.331(3) . ?
F3 C14 1.316(3) . ?

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
C9 Mn1 C8 86.96(9) . . ?
C9 Mn1 N1 93.66(8) . . ?
C8 Mn1 N1 94.16(8) . . ?
C9 Mn1 C10 93.66(8) . . ?
C8 Mn1 C10 94.16(8) . . ?
C9 Mn1 N22 176.38(8) . . ?
C8 Mn1 N22 94.88(8) . . ?
N1 Mn1 N22 83.11(7) . . ?
C10 Mn1 N22 83.11(7) . . ?
C9 Mn1 N12 90.08(8) . . ?
C8 Mn1 N12 177.00(8) . . ?
N1 Mn1 N12 86.55(7) . . ?
C10 Mn1 N12 86.55(7) . . ?
N22 Mn1 N12 88.10(6) . . ?
C9 Mn1 P1 93.20(7) . . ?
C8 Mn1 P1 90.96(6) . . ?
N1 Mn1 P1 171.65(5) . . ?
C10 Mn1 P1 171.65(5) . . ?
N22 Mn1 P1 89.89(5) . . ?
N12 Mn1 P1 88.67(5) . . ?
C41 P1 C31 105.85(9) . . ?
C41 P1 C1 102.59(9) . . ?
C31 P1 C1 99.42(9) . . ?
C41 P1 Mn1 111.81(6) . . ?
C31 P1 Mn1 117.27(6) . . ?
C1 P1 Mn1 118.03(6) . . ?
N12 N11 C11 111.41(16) . . ?
N12 N11 C7 122.09(16) . . ?
C11 N11 C7 124.90(17) . . ?
C13 N12 N11 104.92(16) . . ?
C13 N12 Mn1 129.67(14) . . ?
N11 N12 Mn1 124.86(12) . . ?
C21 N21 N22 111.08(16) . . ?
C21 N21 C7 125.29(16) . . ?
N22 N21 C7 123.42(15) . . ?
C23 N22 N21 105.35(16) . . ?
C23 N22 Mn1 129.05(14) . . ?
N21 N22 Mn1 125.20(12) . . ?
O10 C10 Mn1 165.4(10) . . ?
C15 N1 Mn1 167.5(3) . . ?
N1 C15 C16 179.3(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1 C9 Mn1 177.88(18) . . ?
O2 C8 Mn1 175.19(18) . . ?
N11 C11 C12 107.07(18) . . ?
N11 C11 H11 126.5 . . ?
C12 C11 H11 126.5 . . ?
C11 C12 C13 105.23(18) . . ?
C11 C12 H12 127.4 . . ?
C13 C12 H12 127.4 . . ?
N12 C13 C12 111.35(18) . . ?
N12 C13 H13 124.3 . . ?
C12 C13 H13 124.3 . . ?
N21 C21 C22 107.05(18) . . ?
N21 C21 H21 126.5 . . ?
C22 C21 H21 126.5 . . ?
C21 C22 C23 105.69(18) . . ?
C21 C22 H22 127.2 . . ?
C23 C22 H22 127.2 . . ?
N22 C23 C22 110.80(18) . . ?
N22 C23 H23 124.6 . . ?
C22 C23 H23 124.6 . . ?
C6 C1 C2 117.97(17) . . ?
C6 C1 P1 115.82(15) . . ?
C2 C1 P1 126.19(15) . . ?
C3 C2 C1 119.23(18) . . ?
C3 C2 C7 113.61(17) . . ?
C1 C2 C7 127.15(17) . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.75(19) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 122.19(19) . . ?
C5 C6 H6 118.9 . . ?
C1 C6 H6 118.9 . . ?
N11 C7 N21 111.37(15) . . ?
N11 C7 C2 113.25(16) . . ?
N21 C7 C2 114.77(16) . . ?
N11 C7 H7 105.5 . . ?
N21 C7 H7 105.5 . . ?
C2 C7 H7 105.5 . . ?
C46 C41 C42 118.52(18) . . ?
C46 C41 P1 121.07(15) . . ?
C42 C41 P1 119.81(15) . . ?
C43 C42 C41 120.60(19) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C44 121.0(2) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C45 C44 C43 118.25(19) . . ?
C45 C44 C47 121.1(2) . . ?
C43 C44 C47 120.6(2) . . ?
C44 C45 C46 121.01(19) . . ?
C44 C45 H45 119.5 . . ?
C46 C45 H45 119.5 . . ?
C45 C46 C41 120.56(19) . . ?
C45 C46 H46 119.7 . . ?
C41 C46 H46 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C36 C31 C32 118.27(19) . . ?
C36 C31 P1 117.07(15) . . ?
C32 C31 P1 124.59(15) . . ?
C35 C36 C31 121.08(19) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C36 C35 C34 120.99(19) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C34 C33 118.11(19) . . ?
C35 C34 C37 120.1(2) . . ?
C33 C34 C37 121.8(2) . . ?
C34 C33 C32 121.26(19) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C32 C31 120.27(19) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O5 S3 O4 114.76(10) . . ?
O5 S3 O3 114.85(13) . . ?
O4 S3 O3 115.22(11) . . ?
O5 S3 C14 103.43(12) . . ?
O4 S3 C14 104.27(11) . . ?
O3 S3 C14 101.91(11) . . ?
F3 C14 F2 107.2(2) . . ?
F3 C14 F1 107.9(2) . . ?
F2 C14 F1 107.7(2) . . ?
F3 C14 S3 112.37(18) . . ?
F2 C14 S3 111.04(17) . . ?
F1 C14 S3 110.42(17) . . ?

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
C11 N11 N12 C13 1.5(2) . . . . ?
C7 N11 N12 C13 167.76(17) . . . . ?
C11 N11 N12 Mn1 173.65(13) . . . . ?
C7 N11 N12 Mn1 -20.1(2) . . . . ?
C21 N21 N22 C23 -1.4(2) . . . . ?
C7 N21 N22 C23 -176.33(17) . . . . ?
C21 N21 N22 Mn1 -174.63(13) . . . . ?
C7 N21 N22 Mn1 10.4(2) . . . . ?
N12 N11 C11 C12 -1.3(2) . . . . ?
C7 N11 C11 C12 -167.08(17) . . . . ?
N11 C11 C12 C13 0.5(2) . . . . ?
N11 N12 C13 C12 -1.2(2) . . . . ?
Mn1 N12 C13 C12 -172.76(14) . . . . ?
C11 C12 C13 N12 0.4(2) . . . . ?
N22 N21 C21 C22 0.5(2) . . . . ?
C7 N21 C21 C22 175.34(18) . . . . ?
N21 C21 C22 C23 0.5(2) . . . . ?
N21 N22 C23 C22 1.7(2) . . . . ?
Mn1 N22 C23 C22 174.62(14) . . . . ?
C21 C22 C23 N22 -1.5(2) . . . . ?
C41 P1 C1 C6 54.20(17) . . . . ?
C31 P1 C1 C6 -54.51(16) . . . . ?
Mn1 P1 C1 C6 177.58(13) . . . . ?
C41 P1 C1 C2 -127.90(17) . . . . ?
C31 P1 C1 C2 123.40(18) . . . . ?
Mn1 P1 C1 C2 -4.5(2) . . . . ?
C6 C1 C2 C3 -1.6(3) . . . . ?
P1 C1 C2 C3 -179.43(16) . . . . ?
C6 C1 C2 C7 179.92(18) . . . . ?
P1 C1 C2 C7 2.1(3) . . . . ?
C1 C2 C3 C4 1.3(3) . . . . ?
C7 C2 C3 C4 180.0(2) . . . . ?
C2 C3 C4 C5 -0.3(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
P1 C1 C6 C5 179.10(16) . . . . ?
N12 N11 C7 N21 55.8(2) . . . . ?
C11 N11 C7 N21 -139.92(18) . . . . ?
N12 N11 C7 C2 -75.4(2) . . . . ?
C11 N11 C7 C2 89.0(2) . . . . ?
C21 N21 C7 N11 135.08(19) . . . . ?
N22 N21 C7 N11 -50.7(2) . . . . ?
C21 N21 C7 C2 -94.6(2) . . . . ?
N22 N21 C7 C2 79.6(2) . . . . ?
C3 C2 C7 N11 -113.00(19) . . . . ?
C1 C2 C7 N11 65.6(2) . . . . ?
C3 C2 C7 N21 117.59(19) . . . . ?
C1 C2 C7 N21 -63.8(3) . . . . ?
C31 P1 C41 C46 137.51(16) . . . . ?
C1 P1 C41 C46 33.76(18) . . . . ?
Mn1 P1 C41 C46 -93.68(16) . . . . ?
C31 P1 C41 C42 -51.48(18) . . . . ?
C1 P1 C41 C42 -155.23(16) . . . . ?
Mn1 P1 C41 C42 77.32(17) . . . . ?
C46 C41 C42 C43 -1.7(3) . . . . ?
P1 C41 C42 C43 -172.90(16) . . . . ?
C41 C42 C43 C44 1.9(3) . . . . ?
C42 C43 C44 C45 -1.2(3) . . . . ?
C42 C43 C44 C47 178.1(2) . . . . ?
C43 C44 C45 C46 0.2(3) . . . . ?
C47 C44 C45 C46 -179.0(2) . . . . ?
C44 C45 C46 C41 0.0(3) . . . . ?
C42 C41 C46 C45 0.7(3) . . . . ?
P1 C41 C46 C45 171.86(16) . . . . ?
C41 P1 C31 C36 172.01(15) . . . . ?
C1 P1 C31 C36 -81.93(16) . . . . ?
Mn1 P1 C31 C36 46.49(17) . . . . ?
C41 P1 C31 C32 -11.10(19) . . . . ?
C1 P1 C31 C32 94.96(17) . . . . ?
Mn1 P1 C31 C32 -136.62(15) . . . . ?
C32 C31 C36 C35 -0.3(3) . . . . ?
P1 C31 C36 C35 176.81(15) . . . . ?
C31 C36 C35 C34 0.4(3) . . . . ?
C36 C35 C34 C33 0.2(3) . . . . ?
C36 C35 C34 C37 179.64(19) . . . . ?
C35 C34 C33 C32 -0.8(3) . . . . ?
C37 C34 C33 C32 179.73(19) . . . . ?
C34 C33 C32 C31 0.9(3) . . . . ?
C36 C31 C32 C33 -0.3(3) . . . . ?
P1 C31 C32 C33 -177.20(15) . . . . ?
O5 S3 C14 F3 -60.0(2) . . . . ?
O4 S3 C14 F3 60.3(2) . . . . ?
O3 S3 C14 F3 -179.49(19) . . . . ?
O5 S3 C14 F2 179.91(18) . . . . ?
O4 S3 C14 F2 -59.8(2) . . . . ?
O3 S3 C14 F2 60.4(2) . . . . ?
O5 S3 C14 F1 60.5(2) . . . . ?
O4 S3 C14 F1 -179.16(17) . . . . ?
O3 S3 C14 F1 -59.0(2) . . . . ?

_refine_diff_density_max         0.502
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.057



####################################################################### 
# 
# 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_3-Mn0p92_2-Mn0p08_GARD27D
_database_code_depnum_ccdc_archive 'CCDC 2383876'
loop_
_audit_author_name
_audit_author_address
'Alexander N Erickson'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-09-12 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_id_orcid   
;
0009-0007-5837-0978
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30.92 H27.77 Mn N4.92 O2.08 P, C F3 O3 S'
_chemical_formula_sum            'C31.92 H27.77 F3 Mn N4.92 O5.08 P S'
_chemical_formula_weight         736.57

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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   16.4795(2)
_cell_length_b                   12.8391(2)
_cell_length_c                   16.5133(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.4813(18)
_cell_angle_gamma                90
_cell_volume                     3251.19(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9477
_cell_measurement_theta_min      5.87
_cell_measurement_theta_max      79.12
_exptl_crystal_description       Plate
_exptl_crystal_colour            'Translucent Yellow'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             1510
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    4.949
_shelx_estimated_absorpt_T_min   0.329
_shelx_estimated_absorpt_T_max   0.622
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.3676
_exptl_absorpt_correction_T_max  0.5553
_exptl_absorpt_process_details   
;
SADABS-2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & 
Stalke D. (2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_recrystallization_method 
'Crystals were grown by vapor diffusion of diethyl ether into acetonitrile at ambient temperature in a closed vial.'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  'HELIOS Multi-layer'
_diffrn_source                   'Incoatec micro-focus sealed X-ray tube'
_diffrn_source_type              'I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_source_current           1.1
_diffrn_measurement_device_type  'Bruker D8 Venture, Single Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support 'MiTeGen Dual Thickness MicroMount'
_diffrn_measurement_ambient_temperature_device_make 'Oxford CryoStream 1000'
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_type            'PhotonIII C14'
_diffrn_detector_details         
'charge-integrating and photon counting pixel array'
_diffrn_detector_area_resol_mean 7.41
_diffrn_reflns_number            151831
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.241
_diffrn_reflns_theta_max         80.833
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7086
_reflns_number_gt                7045
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX-5 v2023.9-4 (Bruker, 2024)'
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2024)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    
'ShelXle v6.4.0 Rev1506 (Hübschle et al, 2011)'
_computing_publication_material  
;
CIFTAB-2014/2 (Sheldrick, 2008) and
FinalCif v136 (Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html)
;
_refine_special_details          
;
The initial refinement of the structure determined there was additional electron 
density around the CH3CN molecule (N1 C15 C16), this was initially ignored as it 
was less than 10% contribution. After further consideration, we have decided to 
model this additional density as partially occupied CO. The occupancies of both 
the CO and CH3CN were constrained to a sum of 1 and refined to 0.923(4) for the 
major component (N1 C15 C16) and 0.077(4) for the minor component (C10 O10). 
SADI was used for C10 and O10 to keep the bonding appropriate. Additionally, 
C10 and O10 of the CO molecule and N1 of the CH3CN had their displacement 
parameters constrained with EADP.  

Further investigation has determined that the triflate molecule 
(C14 F1 F2 F3 S3 O3 O4 O5) was disordered across two sites. The occupancies of 
both components were constrained to a sum of 1 and refined to 0.72(2) for the 
major component (C14 F1 F2 F3 S3 O3 O4 O5) and 0.28(2) for the minor component 
(C14A F1A F2A F3A S3A O3A O4A O5A). The minor component was further restrained 
with SIMU and RIGU. 

All hydrogen atoms were placed in calculated positions and had their thermal 
parameters tied to the isotropic thermal parameters of the atoms to which they 
were bonded (1.5x for methyl, 1.2x for others).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+2.0633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7086
_refine_ls_number_parameters     516
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.51384(2) 0.27428(2) 0.29792(2) 0.01159(6) Uani 1 1 d D . . . .
P1 P 0.40285(2) 0.38828(2) 0.28099(2) 0.01118(7) Uani 1 1 d . . . . .
O1 O 0.49047(7) 0.16441(8) 0.44363(6) 0.0231(2) Uani 1 1 d D . . . .
O2 O 0.63536(6) 0.40820(8) 0.43343(6) 0.0240(2) Uani 1 1 d . . . . .
N11 N 0.39146(7) 0.18932(8) 0.12422(7) 0.0134(2) Uani 1 1 d . . . . .
N12 N 0.42564(7) 0.17579(8) 0.21171(7) 0.0136(2) Uani 1 1 d . . . . .
N21 N 0.47902(7) 0.33284(8) 0.11058(7) 0.0133(2) Uani 1 1 d . . . . .
N22 N 0.53396(7) 0.34019(8) 0.19471(7) 0.0136(2) Uani 1 1 d . . . . .
C10 C 0.5961(16) 0.183(2) 0.300(3) 0.0169(3) Uani 0.076(5) 1 d D . P A 1
O10 O 0.6489(7) 0.1219(10) 0.3050(12) 0.0169(3) Uani 0.076(5) 1 d D . P A 1
N1 N 0.60623(13) 0.17502(16) 0.29282(19) 0.0169(3) Uani 0.924(5) 1 d . . P A 2
C15 C 0.65631(11) 0.12666(12) 0.27701(16) 0.0212(4) Uani 0.924(5) 1 d . . P A 2
C16 C 0.72049(11) 0.06490(14) 0.25747(14) 0.0359(5) Uani 0.924(5) 1 d . . P A 2
H16A H 0.779080 0.090748 0.291451 0.054 Uiso 0.924(5) 1 calc R U P A 2
H16B H 0.710129 0.070282 0.195267 0.054 Uiso 0.924(5) 1 calc R U P A 2
H16C H 0.715660 -0.008094 0.272470 0.054 Uiso 0.924(5) 1 calc R U P A 2
C9 C 0.49858(8) 0.20879(10) 0.38633(8) 0.0164(2) Uani 1 1 d D . . . .
C8 C 0.58960(8) 0.35738(10) 0.37819(8) 0.0165(2) Uani 1 1 d . . . . .
C11 C 0.34226(8) 0.10671(10) 0.08355(9) 0.0165(2) Uani 1 1 d . . . . .
H11 H 0.310953 0.099523 0.022780 0.020 Uiso 1 1 calc R U . . .
C12 C 0.34619(9) 0.03553(10) 0.14659(9) 0.0185(3) Uani 1 1 d . . . . .
H12 H 0.318978 -0.030882 0.138840 0.022 Uiso 1 1 calc R U . . .
C13 C 0.39891(8) 0.08171(10) 0.22485(9) 0.0169(2) Uani 1 1 d . . . . .
H13 H 0.413770 0.049946 0.280369 0.020 Uiso 1 1 calc R U . . .
C21 C 0.51403(9) 0.37721(10) 0.05656(9) 0.0178(3) Uani 1 1 d . . . . .
H21 H 0.487642 0.382030 -0.004998 0.021 Uiso 1 1 calc R U . . .
C22 C 0.59489(9) 0.41394(11) 0.10750(9) 0.0194(3) Uani 1 1 d . . . . .
H22 H 0.635386 0.449495 0.088668 0.023 Uiso 1 1 calc R U . . .
C23 C 0.60506(8) 0.38811(10) 0.19257(9) 0.0168(2) Uani 1 1 d . . . . .
H23 H 0.655657 0.402606 0.242282 0.020 Uiso 1 1 calc R U . . .
C1 C 0.32112(8) 0.40821(9) 0.17003(8) 0.0133(2) Uani 1 1 d . . . . .
C2 C 0.32322(8) 0.36428(10) 0.09292(8) 0.0138(2) Uani 1 1 d . . . . .
C3 C 0.25629(9) 0.38752(11) 0.01362(9) 0.0195(3) Uani 1 1 d . . . . .
H3 H 0.257247 0.356730 -0.038339 0.023 Uiso 1 1 calc R U . . .
C4 C 0.18881(9) 0.45425(11) 0.00912(9) 0.0220(3) Uani 1 1 d . . . . .
H4 H 0.144050 0.468989 -0.045322 0.026 Uiso 1 1 calc R U . . .
C5 C 0.18708(9) 0.49937(11) 0.08467(9) 0.0202(3) Uani 1 1 d . . . . .
H5 H 0.141462 0.545898 0.082378 0.024 Uiso 1 1 calc R U . . .
C6 C 0.25254(8) 0.47605(10) 0.16374(8) 0.0167(2) Uani 1 1 d . . . . .
H6 H 0.250758 0.507135 0.215270 0.020 Uiso 1 1 calc R U . . .
C7 C 0.39131(8) 0.28991(10) 0.08430(8) 0.0135(2) Uani 1 1 d . . . . .
H7 H 0.373072 0.275684 0.020554 0.016 Uiso 1 1 calc R U . . .
C41 C 0.33566(8) 0.34818(9) 0.34146(8) 0.0136(2) Uani 1 1 d . . . . .
C42 C 0.36560(8) 0.36379(11) 0.43140(8) 0.0174(2) Uani 1 1 d . . . . .
H42 H 0.417419 0.402618 0.459432 0.021 Uiso 1 1 calc R U . . .
C43 C 0.32003(9) 0.32289(11) 0.47993(9) 0.0202(3) Uani 1 1 d . . . . .
H43 H 0.340031 0.336110 0.540704 0.024 Uiso 1 1 calc R U . . .
C44 C 0.24553(9) 0.26282(11) 0.44120(9) 0.0204(3) Uani 1 1 d . . . . .
C45 C 0.21641(9) 0.24637(11) 0.35187(9) 0.0195(3) Uani 1 1 d . . . . .
H45 H 0.165553 0.205727 0.324298 0.023 Uiso 1 1 calc R U . . .
C46 C 0.26069(8) 0.28858(10) 0.30235(9) 0.0159(2) Uani 1 1 d . . . . .
H46 H 0.239698 0.276729 0.241348 0.019 Uiso 1 1 calc R U . . .
C47 C 0.19864(11) 0.21554(14) 0.49524(11) 0.0318(4) Uani 1 1 d . . . . .
H47A H 0.241403 0.188504 0.549641 0.048 Uiso 1 1 calc R U . . .
H47B H 0.161281 0.158523 0.462805 0.048 Uiso 1 1 calc R U . . .
H47C H 0.162730 0.268823 0.508453 0.048 Uiso 1 1 calc R U . . .
C31 C 0.43221(8) 0.52380(10) 0.31153(8) 0.0136(2) Uani 1 1 d . . . . .
C36 C 0.49348(8) 0.56899(10) 0.28215(8) 0.0163(2) Uani 1 1 d . . . . .
H36 H 0.519578 0.527928 0.250421 0.020 Uiso 1 1 calc R U . . .
C35 C 0.51681(8) 0.67259(11) 0.29852(8) 0.0175(3) Uani 1 1 d . . . . .
H35 H 0.558328 0.701832 0.277556 0.021 Uiso 1 1 calc R U . . .
C34 C 0.48009(9) 0.73452(10) 0.34540(8) 0.0170(3) Uani 1 1 d . . . . .
C33 C 0.41948(9) 0.68956(10) 0.37523(8) 0.0171(2) Uani 1 1 d . . . . .
H33 H 0.394269 0.730526 0.407810 0.020 Uiso 1 1 calc R U . . .
C32 C 0.39508(8) 0.58571(10) 0.35825(8) 0.0160(2) Uani 1 1 d . . . . .
H32 H 0.352947 0.556823 0.378551 0.019 Uiso 1 1 calc R U . . .
C37 C 0.50688(11) 0.84691(11) 0.36306(10) 0.0250(3) Uani 1 1 d . . . . .
H37A H 0.461367 0.885594 0.375250 0.037 Uiso 1 1 calc R U . . .
H37B H 0.515013 0.876953 0.312000 0.037 Uiso 1 1 calc R U . . .
H37C H 0.561688 0.851310 0.413412 0.037 Uiso 1 1 calc R U . . .
S3 S 0.8559(2) 0.3111(2) 0.3433(2) 0.0163(3) Uani 0.724(16) 1 d . . P B 1
F1 F 0.9890(4) 0.3725(6) 0.4775(4) 0.0413(7) Uani 0.724(16) 1 d . . P B 1
F2 F 1.0219(2) 0.3311(4) 0.3683(3) 0.0340(6) Uani 0.724(16) 1 d . . P B 1
F3 F 0.9493(4) 0.4754(5) 0.3689(4) 0.0471(11) Uani 0.724(16) 1 d . . P B 1
O3 O 0.8832(4) 0.2018(6) 0.3750(5) 0.0368(12) Uani 0.724(16) 1 d . . P B 1
O4 O 0.8323(4) 0.3186(6) 0.2492(3) 0.0239(7) Uani 0.724(16) 1 d . . P B 1
O5 O 0.7991(6) 0.3569(6) 0.3788(6) 0.0415(14) Uani 0.724(16) 1 d . . P B 1
C14 C 0.9634(2) 0.3790(3) 0.3929(2) 0.0167(6) Uani 0.724(16) 1 d . . P B 1
S3A S 0.8563(6) 0.2956(7) 0.3460(6) 0.0196(6) Uani 0.276(16) 1 d . U P B 2
F1A F 0.9903(9) 0.3689(11) 0.4798(10) 0.0247(7) Uani 0.276(16) 1 d . U P B 2
F2A F 1.0151(7) 0.3503(8) 0.3585(7) 0.0247(7) Uani 0.276(16) 1 d . U P B 2
F3A F 0.9570(10) 0.4792(11) 0.3716(7) 0.0247(7) Uani 0.276(16) 1 d . U P B 2
O3A O 0.8711(10) 0.2080(15) 0.3829(11) 0.0196(6) Uani 0.276(16) 1 d . U P B 2
O4A O 0.8368(12) 0.3167(14) 0.2596(10) 0.0196(6) Uani 0.276(16) 1 d . U P B 2
O5A O 0.7997(14) 0.3699(13) 0.3776(13) 0.0196(6) Uani 0.276(16) 1 d . U P B 2
C14A C 0.9452(9) 0.3677(10) 0.3862(8) 0.0247(7) Uani 0.276(16) 1 d . U P B 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
Mn1 C9 1.7806(14) . ?
Mn1 C10 1.7810(17) . ?
Mn1 C8 1.8005(14) . ?
Mn1 N1 2.0107(15) . ?
Mn1 N22 2.0359(11) . ?
Mn1 N12 2.0550(11) . ?
Mn1 P1 2.2784(3) . ?
P1 C41 1.8161(13) . ?
P1 C31 1.8268(13) . ?
P1 C1 1.8519(12) . ?
O1 C9 1.1535(17) . ?
O2 C8 1.1501(17) . ?
N11 C11 1.3545(16) . ?
N11 N12 1.3560(14) . ?
N11 C7 1.4495(16) . ?
N12 C13 1.3304(16) . ?
N21 C21 1.3528(16) . ?
N21 N22 1.3554(14) . ?
N21 C7 1.4566(16) . ?
N22 C23 1.3352(16) . ?
C10 O10 1.154(2) . ?
N1 C15 1.137(2) . ?
C15 C16 1.450(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C11 C12 1.3688(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.3978(18) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C21 C22 1.3728(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.3925(19) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C1 C6 1.4002(17) . ?
C1 C2 1.4047(17) . ?
C2 C3 1.4009(17) . ?
C2 C7 1.5193(17) . ?
C3 C4 1.3842(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3881(18) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C41 C46 1.3945(17) . ?
C41 C42 1.3974(17) . ?
C42 C43 1.3866(19) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.390(2) . ?
C44 C47 1.5055(19) . ?
C45 C46 1.3899(18) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C31 C32 1.3955(17) . ?
C31 C36 1.3966(18) . ?
C36 C35 1.3835(19) . ?
C36 H36 0.9500 . ?
C35 C34 1.3930(19) . ?
C35 H35 0.9500 . ?
C34 C33 1.3907(19) . ?
C34 C37 1.5058(18) . ?
C33 C32 1.3912(18) . ?
C33 H33 0.9500 . ?
C32 H32 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
S3 O5 1.403(9) . ?
S3 O4 1.461(5) . ?
S3 O3 1.507(9) . ?
S3 C14 1.872(4) . ?
F1 C14 1.305(7) . ?
F2 C14 1.327(5) . ?
F3 C14 1.294(7) . ?
S3A O3A 1.26(2) . ?
S3A O4A 1.369(16) . ?
S3A O5A 1.55(2) . ?
S3A C14A 1.652(14) . ?
F1A C14A 1.45(2) . ?
F2A C14A 1.405(15) . ?
F3A C14A 1.48(2) . ?

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
C9 Mn1 C10 90.7(17) . . ?
C9 Mn1 C8 86.80(6) . . ?
C10 Mn1 C8 93.3(12) . . ?
C9 Mn1 N1 94.10(9) . . ?
C8 Mn1 N1 94.29(8) . . ?
C9 Mn1 N22 176.27(5) . . ?
C10 Mn1 N22 85.9(17) . . ?
C8 Mn1 N22 95.07(5) . . ?
N1 Mn1 N22 82.55(9) . . ?
C9 Mn1 N12 90.06(5) . . ?
C10 Mn1 N12 87.1(12) . . ?
C8 Mn1 N12 176.84(5) . . ?
N1 Mn1 N12 86.29(7) . . ?
N22 Mn1 N12 88.08(4) . . ?
C9 Mn1 P1 93.20(4) . . ?
C10 Mn1 P1 174.3(16) . . ?
C8 Mn1 P1 91.07(4) . . ?
N1 Mn1 P1 171.16(8) . . ?
N22 Mn1 P1 89.99(3) . . ?
N12 Mn1 P1 88.74(3) . . ?
C41 P1 C31 105.75(6) . . ?
C41 P1 C1 102.37(6) . . ?
C31 P1 C1 99.47(5) . . ?
C41 P1 Mn1 111.97(4) . . ?
C31 P1 Mn1 117.29(4) . . ?
C1 P1 Mn1 118.07(4) . . ?
C11 N11 N12 111.56(10) . . ?
C11 N11 C7 124.83(11) . . ?
N12 N11 C7 121.98(10) . . ?
C13 N12 N11 104.89(10) . . ?
C13 N12 Mn1 129.65(9) . . ?
N11 N12 Mn1 124.87(8) . . ?
C21 N21 N22 111.12(10) . . ?
C21 N21 C7 125.38(11) . . ?
N22 N21 C7 123.32(10) . . ?
C23 N22 N21 105.56(10) . . ?
C23 N22 Mn1 128.84(9) . . ?
N21 N22 Mn1 125.21(8) . . ?
O10 C10 Mn1 176(4) . . ?
C15 N1 Mn1 168.6(3) . . ?
N1 C15 C16 179.6(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1 C9 Mn1 178.09(12) . . ?
O2 C8 Mn1 175.25(12) . . ?
N11 C11 C12 107.02(11) . . ?
N11 C11 H11 126.5 . . ?
C12 C11 H11 126.5 . . ?
C11 C12 C13 105.08(11) . . ?
C11 C12 H12 127.5 . . ?
C13 C12 H12 127.5 . . ?
N12 C13 C12 111.42(12) . . ?
N12 C13 H13 124.3 . . ?
C12 C13 H13 124.3 . . ?
N21 C21 C22 107.05(11) . . ?
N21 C21 H21 126.5 . . ?
C22 C21 H21 126.5 . . ?
C21 C22 C23 105.52(11) . . ?
C21 C22 H22 127.2 . . ?
C23 C22 H22 127.2 . . ?
N22 C23 C22 110.72(12) . . ?
N22 C23 H23 124.6 . . ?
C22 C23 H23 124.6 . . ?
C6 C1 C2 118.02(11) . . ?
C6 C1 P1 115.73(9) . . ?
C2 C1 P1 126.23(9) . . ?
C3 C2 C1 119.31(12) . . ?
C3 C2 C7 113.70(11) . . ?
C1 C2 C7 126.98(11) . . ?
C4 C3 C2 121.60(13) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.45(12) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 119.46(12) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 122.15(12) . . ?
C5 C6 H6 118.9 . . ?
C1 C6 H6 118.9 . . ?
N11 C7 N21 111.43(10) . . ?
N11 C7 C2 113.31(10) . . ?
N21 C7 C2 114.87(10) . . ?
N11 C7 H7 105.4 . . ?
N21 C7 H7 105.4 . . ?
C2 C7 H7 105.4 . . ?
C46 C41 C42 118.62(12) . . ?
C46 C41 P1 121.07(10) . . ?
C42 C41 P1 119.65(9) . . ?
C43 C42 C41 120.31(12) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 121.19(13) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C45 C44 C43 118.39(12) . . ?
C45 C44 C47 121.00(13) . . ?
C43 C44 C47 120.60(14) . . ?
C46 C45 C44 120.90(12) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C41 120.56(12) . . ?
C45 C46 H46 119.7 . . ?
C41 C46 H46 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C32 C31 C36 118.33(11) . . ?
C32 C31 P1 124.73(10) . . ?
C36 C31 P1 116.87(9) . . ?
C35 C36 C31 121.07(12) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C36 C35 C34 120.75(12) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C33 C34 C35 118.32(12) . . ?
C33 C34 C37 121.79(13) . . ?
C35 C34 C37 119.89(13) . . ?
C34 C33 C32 121.24(12) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C32 C31 120.29(12) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O5 S3 O4 117.3(5) . . ?
O5 S3 O3 113.9(4) . . ?
O4 S3 O3 111.1(5) . . ?
O5 S3 C14 106.9(5) . . ?
O4 S3 C14 106.0(3) . . ?
O3 S3 C14 99.6(3) . . ?
F3 C14 F1 109.9(5) . . ?
F3 C14 F2 114.7(5) . . ?
F1 C14 F2 108.1(4) . . ?
F3 C14 S3 106.1(4) . . ?
F1 C14 S3 108.8(4) . . ?
F2 C14 S3 109.0(3) . . ?
O3A S3A O4A 127.6(13) . . ?
O3A S3A O5A 114.8(11) . . ?
O4A S3A O5A 106.7(12) . . ?
O3A S3A C14A 108.6(11) . . ?
O4A S3A C14A 98.3(10) . . ?
O5A S3A C14A 94.3(10) . . ?
F2A C14A F1A 100.8(10) . . ?
F2A C14A F3A 85.8(11) . . ?
F1A C14A F3A 96.7(11) . . ?
F2A C14A S3A 119.5(10) . . ?
F1A C14A S3A 117.9(10) . . ?
F3A C14A S3A 128.9(12) . . ?

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
C11 N11 N12 C13 1.73(14) . . . . ?
C7 N11 N12 C13 167.85(11) . . . . ?
C11 N11 N12 Mn1 173.64(8) . . . . ?
C7 N11 N12 Mn1 -20.24(15) . . . . ?
C21 N21 N22 C23 -1.26(14) . . . . ?
C7 N21 N22 C23 -176.69(11) . . . . ?
C21 N21 N22 Mn1 -174.65(9) . . . . ?
C7 N21 N22 Mn1 9.91(16) . . . . ?
N12 N11 C11 C12 -1.50(14) . . . . ?
C7 N11 C11 C12 -167.14(11) . . . . ?
N11 C11 C12 C13 0.63(15) . . . . ?
N11 N12 C13 C12 -1.30(14) . . . . ?
Mn1 N12 C13 C12 -172.68(9) . . . . ?
C11 C12 C13 N12 0.43(15) . . . . ?
N22 N21 C21 C22 0.47(15) . . . . ?
C7 N21 C21 C22 175.79(12) . . . . ?
N21 C21 C22 C23 0.49(15) . . . . ?
N21 N22 C23 C22 1.57(14) . . . . ?
Mn1 N22 C23 C22 174.63(9) . . . . ?
C21 C22 C23 N22 -1.31(15) . . . . ?
C41 P1 C1 C6 54.26(11) . . . . ?
C31 P1 C1 C6 -54.30(10) . . . . ?
Mn1 P1 C1 C6 177.70(8) . . . . ?
C41 P1 C1 C2 -127.57(11) . . . . ?
C31 P1 C1 C2 123.88(11) . . . . ?
Mn1 P1 C1 C2 -4.13(13) . . . . ?
C6 C1 C2 C3 -1.56(18) . . . . ?
P1 C1 C2 C3 -179.70(10) . . . . ?
C6 C1 C2 C7 179.51(12) . . . . ?
P1 C1 C2 C7 1.37(19) . . . . ?
C1 C2 C3 C4 1.1(2) . . . . ?
C7 C2 C3 C4 -179.79(12) . . . . ?
C2 C3 C4 C5 0.0(2) . . . . ?
C3 C4 C5 C6 -0.7(2) . . . . ?
C4 C5 C6 C1 0.2(2) . . . . ?
C2 C1 C6 C5 0.91(19) . . . . ?
P1 C1 C6 C5 179.24(10) . . . . ?
C11 N11 C7 N21 -139.83(12) . . . . ?
N12 N11 C7 N21 55.94(15) . . . . ?
C11 N11 C7 C2 88.79(14) . . . . ?
N12 N11 C7 C2 -75.44(14) . . . . ?
C21 N21 C7 N11 134.65(12) . . . . ?
N22 N21 C7 N11 -50.58(15) . . . . ?
C21 N21 C7 C2 -94.78(14) . . . . ?
N22 N21 C7 C2 80.00(14) . . . . ?
C3 C2 C7 N11 -112.77(12) . . . . ?
C1 C2 C7 N11 66.21(16) . . . . ?
C3 C2 C7 N21 117.57(12) . . . . ?
C1 C2 C7 N21 -63.45(16) . . . . ?
C31 P1 C41 C46 137.79(10) . . . . ?
C1 P1 C41 C46 34.08(11) . . . . ?
Mn1 P1 C41 C46 -93.36(10) . . . . ?
C31 P1 C41 C42 -51.65(11) . . . . ?
C1 P1 C41 C42 -155.36(10) . . . . ?
Mn1 P1 C41 C42 77.20(11) . . . . ?
C46 C41 C42 C43 -1.67(19) . . . . ?
P1 C41 C42 C43 -172.46(10) . . . . ?
C41 C42 C43 C44 2.1(2) . . . . ?
C42 C43 C44 C45 -1.4(2) . . . . ?
C42 C43 C44 C47 177.68(13) . . . . ?
C43 C44 C45 C46 0.2(2) . . . . ?
C47 C44 C45 C46 -178.85(13) . . . . ?
C44 C45 C46 C41 0.2(2) . . . . ?
C42 C41 C46 C45 0.50(19) . . . . ?
P1 C41 C46 C45 171.16(10) . . . . ?
C41 P1 C31 C32 -11.07(12) . . . . ?
C1 P1 C31 C32 94.76(11) . . . . ?
Mn1 P1 C31 C32 -136.72(10) . . . . ?
C41 P1 C31 C36 171.95(10) . . . . ?
C1 P1 C31 C36 -82.23(10) . . . . ?
Mn1 P1 C31 C36 46.30(11) . . . . ?
C32 C31 C36 C35 -0.22(19) . . . . ?
P1 C31 C36 C35 176.96(10) . . . . ?
C31 C36 C35 C34 0.4(2) . . . . ?
C36 C35 C34 C33 -0.02(19) . . . . ?
C36 C35 C34 C37 179.55(12) . . . . ?
C35 C34 C33 C32 -0.64(19) . . . . ?
C37 C34 C33 C32 179.80(12) . . . . ?
C34 C33 C32 C31 0.87(19) . . . . ?
C36 C31 C32 C33 -0.43(18) . . . . ?
P1 C31 C32 C33 -177.37(10) . . . . ?
O5 S3 C14 F3 -62.5(5) . . . . ?
O4 S3 C14 F3 63.4(5) . . . . ?
O3 S3 C14 F3 178.8(5) . . . . ?
O5 S3 C14 F1 55.8(6) . . . . ?
O4 S3 C14 F1 -178.4(5) . . . . ?
O3 S3 C14 F1 -63.0(6) . . . . ?
O5 S3 C14 F2 173.5(5) . . . . ?
O4 S3 C14 F2 -60.6(4) . . . . ?
O3 S3 C14 F2 54.7(6) . . . . ?
O3A S3A C14A F2A 77.6(13) . . . . ?
O4A S3A C14A F2A -56.9(13) . . . . ?
O5A S3A C14A F2A -164.4(11) . . . . ?
O3A S3A C14A F1A -45.4(15) . . . . ?
O4A S3A C14A F1A -179.8(13) . . . . ?
O5A S3A C14A F1A 72.6(13) . . . . ?
O3A S3A C14A F3A -172.1(12) . . . . ?
O4A S3A C14A F3A 53.5(16) . . . . ?
O5A S3A C14A F3A -54.1(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C16^b H16A^b S3A^b 0.98 2.92 3.677(9) 135.2 . yes
C16^b H16A^b O3A^b 0.98 2.27 3.172(19) 151.9 . yes
C16^b H16C^b O4A^b 0.98 2.40 3.306(19) 153.8 2_645 yes
C11 H11 O5^a 0.95 2.38 3.224(9) 147.8 4_565 yes
C11 H11 O5A^b 0.95 2.37 3.23(2) 149.8 4_565 yes
C21 H21 O3^a 0.95 2.36 3.151(7) 141.0 4_565 yes
C21 H21 O3A^b 0.95 2.42 3.166(19) 135.4 4_565 yes
C23 H23 O5A^b 0.95 2.63 3.54(2) 159.4 . yes
C7 H7 O3^a 1.00 2.49 3.411(8) 153.6 4_565 yes
C7 H7 S3A^b 1.00 2.94 3.919(10) 166.7 4_565 yes
C7 H7 O3A^b 1.00 2.27 3.219(16) 157.7 4_565 yes
C36 H36 N22 0.95 2.62 3.4446(17) 145.2 . yes

_refine_diff_density_max         0.317
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.049




####################################################################### 
# 
# 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_3-Re_gard25u
_database_code_depnum_ccdc_archive 'CCDC 2371551'
loop_
_audit_author_name
_audit_author_address
'James Gardinier'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_audit_creation_date             2024-03-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/1
loop_
_audit_author_email
james.gardinier@marquette.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H28 N5 O2 P Re, C F3 O3 S'
_chemical_formula_sum            'C32 H28 F3 N5 O5 P Re S'
_chemical_formula_weight         868.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         C32H25N5F3O5PSRe
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'
F F 0.0727 0.0534 '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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   16.6364(3)
_cell_length_b                   12.9137(2)
_cell_length_c                   16.6780(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.962(2)
_cell_angle_gamma                90
_cell_volume                     3323.04(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12601
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.5300
_cell_measurement_theta_min      4.4170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.766
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 0 9 0.0289
9 0 -9 0.0269
7 0 4 0.1337
-7 0 -4 0.1337
-7 5 7 0.0837
7 -5 -7 0.0587
-3 4 10 0.0427
6 -4 5 0.1400

_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.056
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
-8.9999 0.0000 9.0000 0.6665 -0.0527 0.7492
8.9999 -0.0000 -9.0000 -0.6665 0.0527 -0.7492
7.0000 -0.0000 4.0000 -0.2735 0.8805 0.0786
-7.0000 0.0000 -4.0000 0.2735 -0.8805 -0.0786
-6.9999 5.0000 7.0000 0.0849 -0.2082 0.9563
6.9999 -5.0000 -7.0000 -0.0849 0.2082 -0.9563
-2.9999 4.0000 10.0000 0.0312 0.3828 0.9694
6.0000 -4.0000 5.0000 0.1473 1.0084 -0.1371

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.607
_diffrn_reflns_theta_min         4.460
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  32.00   1.00    1.00    --  -42.46  37.00 -30.00   99
  2  ω    -92.00  -2.00   1.00    1.00    --  -42.46 125.00 -30.00   90
  3  ω     23.00  98.00   1.00    1.00    --   42.46-125.00-180.00   75
  4  ω     17.00 110.00   1.00    2.50    --  100.00 -94.00-120.00   93
  5  ω     94.00 173.00   1.00    2.50    --  100.00 125.00-150.00   79
  6  ω     27.00 118.00   1.00    2.50    --  100.00-125.00-150.00   91
  7  ω     72.00 176.00   1.00    2.50    --  100.00  30.00 120.00  104
  8  ω     47.00 178.00   1.00    2.50    --  100.00  15.00  30.00  131
  9  ω     27.00 126.00   1.00    2.50    --  100.00 -45.00 -60.00   99
 10  ω     18.00 153.00   1.00    2.50    --  100.00 -15.00 150.00  135
 11  ω   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00  30.00  109
 12  ω     10.00 119.00   1.00    1.00    --   42.46  77.00 -90.00  109
 13  ω     14.00 116.00   1.00    1.00    --   42.46  57.00-180.00  102
 14  ω     71.00 132.00   1.00    2.50    --  100.00  61.00 150.00   61
 15  ω     47.00 178.00   1.00    2.50    --  100.00  15.00 -90.00  131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517969000
_diffrn_orient_matrix_UB_12      -0.0866965000
_diffrn_orient_matrix_UB_13      0.0222580000
_diffrn_orient_matrix_UB_21      0.0821701000
_diffrn_orient_matrix_UB_22      -0.0334554000
_diffrn_orient_matrix_UB_23      0.0763169000
_diffrn_orient_matrix_UB_31      -0.0231255000
_diffrn_orient_matrix_UB_32      0.0747272000
_diffrn_orient_matrix_UB_33      0.0601147000
_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                5398
_reflns_number_total             6303
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.142
_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     436
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0345
_refine_ls_restrained_S_all      1.052
_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)+(0.0501P)²+1.8456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0897
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C7(H7)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
1.c Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C47(H47a,H47b,H47c), C16(H16a,H16b,H16c)
;
_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 0.51667(2) 0.72885(2) 0.80459(2) 0.01275(8) Uani 1 1 d . . . . .
P1 P 0.40210(6) 0.61277(8) 0.78545(7) 0.0132(2) Uani 1 1 d . . . . .
O1 O 0.6416(2) 0.5850(3) 0.9410(2) 0.0255(7) Uani 1 1 d . . . . .
O2 O 0.4858(2) 0.8444(3) 0.9505(2) 0.0246(7) Uani 1 1 d . . . . .
N1 N 0.6128(2) 0.8320(3) 0.7976(2) 0.0178(8) Uani 1 1 d . . . . .
N11 N 0.3915(2) 0.8146(3) 0.6235(2) 0.0155(7) Uani 1 1 d . . . . .
N12 N 0.4268(2) 0.8326(3) 0.7100(2) 0.0132(7) Uani 1 1 d . . . . .
N21 N 0.4784(2) 0.6690(3) 0.6113(2) 0.0149(7) Uani 1 1 d . . . . .
N22 N 0.5359(2) 0.6620(3) 0.6945(2) 0.0151(7) Uani 1 1 d . . . . .
C1 C 0.3213(3) 0.5940(3) 0.6736(3) 0.0157(9) Uani 1 1 d . . . . .
C2 C 0.3234(3) 0.6381(3) 0.5973(3) 0.0145(8) Uani 1 1 d . . . . .
C3 C 0.2565(3) 0.6156(4) 0.5187(3) 0.0199(9) Uani 1 1 d . . . . .
H3 H 0.257358 0.645386 0.468304 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1887(3) 0.5502(4) 0.5138(3) 0.0227(10) Uani 1 1 d . . . . .
H4 H 0.144735 0.536631 0.460727 0.027 Uiso 1 1 calc R U . . .
C5 C 0.1873(3) 0.5053(4) 0.5887(3) 0.0222(10) Uani 1 1 d . . . . .
H5 H 0.142680 0.460589 0.586438 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2531(3) 0.5277(4) 0.6671(3) 0.0194(9) Uani 1 1 d . . . . .
H6 H 0.251643 0.497382 0.717089 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3902(3) 0.7118(3) 0.5865(3) 0.0149(9) Uani 1 1 d . . . . .
H7 H 0.370681 0.723519 0.523995 0.018 Uiso 1 1 calc R U . . .
C8 C 0.5958(3) 0.6387(4) 0.8884(3) 0.0188(9) Uani 1 1 d . . . . .
C9 C 0.4979(3) 0.7988(3) 0.8956(3) 0.0165(9) Uani 1 1 d . . . . .
C11 C 0.3420(3) 0.8947(3) 0.5815(3) 0.0194(9) Uani 1 1 d . . . . .
H11 H 0.310504 0.899009 0.522329 0.023 Uiso 1 1 calc R U . . .
C12 C 0.3466(3) 0.9689(3) 0.6417(3) 0.0194(9) Uani 1 1 d . . . . .
H12 H 0.319704 1.033406 0.632171 0.023 Uiso 1 1 calc R U . . .
C13 C 0.4004(3) 0.9264(3) 0.7206(3) 0.0187(9) Uani 1 1 d . . . . .
H13 H 0.415763 0.959765 0.773693 0.022 Uiso 1 1 calc R U . . .
C15 C 0.6617(3) 0.8797(4) 0.7802(3) 0.0234(10) Uani 1 1 d . . . . .
C16 C 0.7237(3) 0.9415(4) 0.7583(4) 0.0392(14) Uani 1 1 d . . . . .
H16a H 0.708707 0.940201 0.696840 0.059 Uiso 1 1 calc R U . . .
H16b H 0.780781 0.913366 0.786638 0.059 Uiso 1 1 calc R U . . .
H16c H 0.722492 1.011574 0.776940 0.059 Uiso 1 1 calc R U . . .
C21 C 0.5097(3) 0.6243(3) 0.5560(3) 0.0190(9) Uani 1 1 d . . . . .
H21 H 0.481742 0.618976 0.496383 0.023 Uiso 1 1 calc R U . . .
C22 C 0.5910(3) 0.5880(4) 0.6050(3) 0.0202(9) Uani 1 1 d . . . . .
H22 H 0.628861 0.552884 0.585238 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6052(3) 0.6147(3) 0.6900(3) 0.0170(9) Uani 1 1 d . . . . .
H23 H 0.655950 0.601236 0.737165 0.020 Uiso 1 1 calc R U . . .
C31 C 0.3350(3) 0.6519(3) 0.8450(3) 0.0161(9) Uani 1 1 d . . . . .
C32 C 0.3638(3) 0.6355(3) 0.9335(3) 0.0185(9) Uani 1 1 d . . . . .
H32 H 0.413267 0.595970 0.960834 0.022 Uiso 1 1 calc R U . . .
C33 C 0.3193(3) 0.6777(4) 0.9817(3) 0.0218(10) Uani 1 1 d . . . . .
H33 H 0.338809 0.664855 1.040789 0.026 Uiso 1 1 calc R U . . .
C34 C 0.2461(3) 0.7389(4) 0.9431(3) 0.0223(10) Uani 1 1 d . . . . .
C35 C 0.2175(3) 0.7554(4) 0.8539(3) 0.0232(10) Uani 1 1 d . . . . .
H35 H 0.168667 0.796091 0.826840 0.028 Uiso 1 1 calc R U . . .
C36 C 0.2603(3) 0.7124(3) 0.8050(3) 0.0181(9) Uani 1 1 d . . . . .
H36 H 0.239609 0.723531 0.745670 0.022 Uiso 1 1 calc R U . . .
C37 C 0.2000(3) 0.7875(4) 0.9960(4) 0.0315(12) Uani 1 1 d . . . . .
H37a H 0.166570 0.735729 1.010948 0.047 Uiso 1 1 calc R U . . .
H37b H 0.162283 0.841290 0.963101 0.047 Uiso 1 1 calc R U . . .
H37c H 0.241935 0.816346 1.047884 0.047 Uiso 1 1 calc R U . . .
C41 C 0.4317(3) 0.4771(3) 0.8138(3) 0.0159(9) Uani 1 1 d . . . . .
C42 C 0.4923(3) 0.4347(3) 0.7838(3) 0.0187(9) Uani 1 1 d . . . . .
H42 H 0.517145 0.476015 0.753577 0.022 Uiso 1 1 calc R U . . .
C43 C 0.5158(3) 0.3312(4) 0.7988(3) 0.0199(9) Uani 1 1 d . . . . .
H43 H 0.556084 0.303915 0.778184 0.024 Uiso 1 1 calc R U . . .
C44 C 0.4804(3) 0.2681(3) 0.8437(3) 0.0186(9) Uani 1 1 d . . . . .
C45 C 0.4202(3) 0.3106(4) 0.8740(3) 0.0190(9) Uani 1 1 d . . . . .
H45 H 0.396058 0.269238 0.904793 0.023 Uiso 1 1 calc R U . . .
C46 C 0.3954(3) 0.4139(3) 0.8590(3) 0.0182(9) Uani 1 1 d . . . . .
H46 H 0.354641 0.440792 0.879141 0.022 Uiso 1 1 calc R U . . .
C47 C 0.5076(3) 0.1556(4) 0.8598(3) 0.0255(10) Uani 1 1 d . . . . .
H47a H 0.508439 0.125457 0.807507 0.038 Uiso 1 1 calc R U . . .
H47b H 0.467236 0.118751 0.877899 0.038 Uiso 1 1 calc R U . . .
H47c H 0.564481 0.151477 0.904186 0.038 Uiso 1 1 calc R U . . .
S1 S 0.35402(7) 0.80508(9) 0.34502(7) 0.0205(2) Uani 1 1 d . . . . .
F1 F 0.45102(19) 0.9713(2) 0.3679(2) 0.0405(8) Uani 1 1 d . . . . .
F2 F 0.48682(19) 0.8701(3) 0.47830(19) 0.0355(7) Uani 1 1 d . . . . .
F3 F 0.51789(18) 0.8292(3) 0.3687(2) 0.0395(8) Uani 1 1 d . . . . .
O3 O 0.3326(2) 0.8117(3) 0.2532(2) 0.0258(7) Uani 1 1 d . . . . .
O4 O 0.2983(2) 0.8630(3) 0.3764(2) 0.0333(8) Uani 1 1 d . . . . .
O5 O 0.3747(2) 0.7028(3) 0.3815(2) 0.0382(10) Uani 1 1 d . . . . .
C14 C 0.4583(3) 0.8723(4) 0.3924(3) 0.0242(10) 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
Re1 P1 2.3510(10) . ?
Re1 N1 2.118(4) . ?
Re1 N12 2.180(3) . ?
Re1 N22 2.158(4) . ?
Re1 C8 1.914(5) . ?
Re1 C9 1.890(5) . ?
P1 C1 1.863(4) . ?
P1 C31 1.821(4) . ?
P1 C41 1.833(4) . ?
O1 C8 1.154(6) . ?
O2 C9 1.167(6) . ?
N1 C15 1.141(6) . ?
N11 N12 1.358(5) . ?
N11 C7 1.461(5) . ?
N11 C11 1.344(6) . ?
N12 C13 1.324(6) . ?
N21 N22 1.363(5) . ?
N21 C7 1.474(5) . ?
N21 C21 1.347(6) . ?
N22 C23 1.331(5) . ?
C1 C2 1.406(6) . ?
C1 C6 1.393(6) . ?
C2 C3 1.397(6) . ?
C2 C7 1.524(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.369(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.398(6) . ?
C13 H13 0.9300 . ?
C15 C16 1.453(7) . ?
C16 H16a 0.9600 . ?
C16 H16b 0.9600 . ?
C16 H16c 0.9600 . ?
C21 H21 0.9300 . ?
C21 C22 1.375(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.392(6) . ?
C23 H23 0.9300 . ?
C31 C32 1.387(6) . ?
C31 C36 1.407(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.393(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.391(7) . ?
C34 C35 1.398(7) . ?
C34 C37 1.506(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.383(7) . ?
C36 H36 0.9300 . ?
C37 H37a 0.9600 . ?
C37 H37b 0.9600 . ?
C37 H37c 0.9600 . ?
C41 C42 1.395(6) . ?
C41 C46 1.391(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.389(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.378(7) . ?
C44 C45 1.392(7) . ?
C44 C47 1.515(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.391(6) . ?
C46 H46 0.9300 . ?
C47 H47a 0.9600 . ?
C47 H47b 0.9600 . ?
C47 H47c 0.9600 . ?
S1 O3 1.439(3) . ?
S1 O4 1.434(4) . ?
S1 O5 1.441(4) . ?
S1 C14 1.834(5) . ?
F1 C14 1.334(6) . ?
F2 C14 1.330(6) . ?
F3 C14 1.320(6) . ?

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
N1 Re1 P1 169.78(10) . . ?
N1 Re1 N12 84.33(13) . . ?
N1 Re1 N22 81.33(14) . . ?
N12 Re1 P1 89.53(9) . . ?
N22 Re1 P1 90.01(9) . . ?
N22 Re1 N12 84.82(13) . . ?
C8 Re1 P1 90.69(13) . . ?
C8 Re1 N1 95.51(16) . . ?
C8 Re1 N12 179.53(16) . . ?
C8 Re1 N22 95.60(16) . . ?
C9 Re1 P1 92.56(13) . . ?
C9 Re1 N1 95.67(16) . . ?
C9 Re1 N12 90.79(15) . . ?
C9 Re1 N22 174.89(15) . . ?
C9 Re1 C8 88.79(18) . . ?
C1 P1 Re1 117.62(14) . . ?
C31 P1 Re1 112.37(14) . . ?
C31 P1 C1 102.82(19) . . ?
C31 P1 C41 106.5(2) . . ?
C41 P1 Re1 116.66(13) . . ?
C41 P1 C1 99.07(19) . . ?
C15 N1 Re1 168.1(4) . . ?
N12 N11 C7 122.4(3) . . ?
C11 N11 N12 111.1(4) . . ?
C11 N11 C7 124.7(4) . . ?
N11 N12 Re1 124.8(3) . . ?
C13 N12 Re1 129.6(3) . . ?
C13 N12 N11 105.4(3) . . ?
N22 N21 C7 123.9(3) . . ?
C21 N21 N22 111.3(3) . . ?
C21 N21 C7 124.6(4) . . ?
N21 N22 Re1 124.6(3) . . ?
C23 N22 Re1 129.7(3) . . ?
C23 N22 N21 105.5(3) . . ?
C2 C1 P1 126.9(3) . . ?
C6 C1 P1 114.8(3) . . ?
C6 C1 C2 118.3(4) . . ?
C1 C2 C7 128.8(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C7 112.3(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 121.9(4) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(4) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.3(4) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 H6 118.8 . . ?
C5 C6 C1 122.3(4) . . ?
C5 C6 H6 118.8 . . ?
N11 C7 N21 111.5(3) . . ?
N11 C7 C2 114.4(3) . . ?
N11 C7 H7 104.8 . . ?
N21 C7 C2 115.2(3) . . ?
N21 C7 H7 104.8 . . ?
C2 C7 H7 104.8 . . ?
O1 C8 Re1 177.2(4) . . ?
O2 C9 Re1 178.1(4) . . ?
N11 C11 H11 126.2 . . ?
N11 C11 C12 107.6(4) . . ?
C12 C11 H11 126.2 . . ?
C11 C12 H12 127.6 . . ?
C11 C12 C13 104.8(4) . . ?
C13 C12 H12 127.6 . . ?
N12 C13 C12 111.2(4) . . ?
N12 C13 H13 124.4 . . ?
C12 C13 H13 124.4 . . ?
N1 C15 C16 179.4(6) . . ?
C15 C16 H16a 109.5 . . ?
C15 C16 H16b 109.5 . . ?
C15 C16 H16c 109.5 . . ?
H16a C16 H16b 109.5 . . ?
H16a C16 H16c 109.5 . . ?
H16b C16 H16c 109.5 . . ?
N21 C21 H21 126.7 . . ?
N21 C21 C22 106.7(4) . . ?
C22 C21 H21 126.7 . . ?
C21 C22 H22 127.0 . . ?
C21 C22 C23 105.9(4) . . ?
C23 C22 H22 127.0 . . ?
N22 C23 C22 110.6(4) . . ?
N22 C23 H23 124.7 . . ?
C22 C23 H23 124.7 . . ?
C32 C31 P1 119.9(3) . . ?
C32 C31 C36 118.7(4) . . ?
C36 C31 P1 120.6(3) . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.5(4) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.2(4) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C35 118.0(4) . . ?
C33 C34 C37 120.9(5) . . ?
C35 C34 C37 121.0(5) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.3(4) . . ?
C36 C35 H35 119.3 . . ?
C31 C36 H36 119.9 . . ?
C35 C36 C31 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C34 C37 H37a 109.5 . . ?
C34 C37 H37b 109.5 . . ?
C34 C37 H37c 109.5 . . ?
H37a C37 H37b 109.5 . . ?
H37a C37 H37c 109.5 . . ?
H37b C37 H37c 109.5 . . ?
C42 C41 P1 116.3(3) . . ?
C46 C41 P1 124.8(3) . . ?
C46 C41 C42 118.8(4) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.3(4) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(4) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 C45 118.4(4) . . ?
C43 C44 C47 120.2(4) . . ?
C45 C44 C47 121.5(4) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 C44 121.2(4) . . ?
C46 C45 H45 119.4 . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.1(4) . . ?
C45 C46 H46 120.0 . . ?
C44 C47 H47a 109.5 . . ?
C44 C47 H47b 109.5 . . ?
C44 C47 H47c 109.5 . . ?
H47a C47 H47b 109.5 . . ?
H47a C47 H47c 109.5 . . ?
H47b C47 H47c 109.5 . . ?
O3 S1 O5 115.4(2) . . ?
O3 S1 C14 104.4(2) . . ?
O4 S1 O3 114.9(2) . . ?
O4 S1 O5 114.1(2) . . ?
O4 S1 C14 103.5(2) . . ?
O5 S1 C14 102.3(2) . . ?
F1 C14 S1 111.0(3) . . ?
F2 C14 S1 110.7(3) . . ?
F2 C14 F1 107.8(4) . . ?
F3 C14 S1 111.5(3) . . ?
F3 C14 F1 107.7(4) . . ?
F3 C14 F2 108.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 P1 C1 C2 3.5(4) . . . . ?
Re1 P1 C1 C6 -177.4(3) . . . . ?
Re1 P1 C31 C32 -77.2(4) . . . . ?
Re1 P1 C31 C36 93.2(3) . . . . ?
Re1 P1 C41 C42 -45.9(4) . . . . ?
Re1 P1 C41 C46 137.1(3) . . . . ?
Re1 N12 C13 C12 176.2(3) . . . . ?
Re1 N22 C23 C22 -177.0(3) . . . . ?
P1 C1 C2 C3 -179.6(3) . . . . ?
P1 C1 C2 C7 -0.6(6) . . . . ?
P1 C1 C6 C5 179.9(4) . . . . ?
P1 C31 C32 C33 170.9(3) . . . . ?
P1 C31 C36 C35 -169.8(3) . . . . ?
P1 C41 C42 C43 -177.1(3) . . . . ?
P1 C41 C46 C45 177.3(3) . . . . ?
N11 N12 C13 C12 1.3(5) . . . . ?
N11 C11 C12 C13 -0.7(5) . . . . ?
N12 N11 C7 N21 -57.6(5) . . . . ?
N12 N11 C7 C2 75.2(5) . . . . ?
N12 N11 C11 C12 1.5(5) . . . . ?
N21 N22 C23 C22 -2.2(5) . . . . ?
N21 C21 C22 C23 -0.6(5) . . . . ?
N22 N21 C7 N11 52.7(5) . . . . ?
N22 N21 C7 C2 -79.7(5) . . . . ?
N22 N21 C21 C22 -0.8(5) . . . . ?
C1 P1 C31 C32 155.3(4) . . . . ?
C1 P1 C31 C36 -34.3(4) . . . . ?
C1 P1 C41 C42 81.4(3) . . . . ?
C1 P1 C41 C46 -95.6(4) . . . . ?
C1 C2 C3 C4 -0.8(6) . . . . ?
C1 C2 C7 N11 -67.5(5) . . . . ?
C1 C2 C7 N21 63.6(6) . . . . ?
C2 C1 C6 C5 -0.9(6) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C3 C2 C7 N11 111.5(4) . . . . ?
C3 C2 C7 N21 -117.4(4) . . . . ?
C3 C4 C5 C6 0.7(7) . . . . ?
C4 C5 C6 C1 -0.1(7) . . . . ?
C6 C1 C2 C3 1.4(6) . . . . ?
C6 C1 C2 C7 -179.7(4) . . . . ?
C7 N11 N12 Re1 17.6(5) . . . . ?
C7 N11 N12 C13 -167.2(4) . . . . ?
C7 N11 C11 C12 166.6(4) . . . . ?
C7 N21 N22 Re1 -8.2(5) . . . . ?
C7 N21 N22 C23 176.7(4) . . . . ?
C7 N21 C21 C22 -175.6(4) . . . . ?
C7 C2 C3 C4 -179.9(4) . . . . ?
C11 N11 N12 Re1 -176.9(3) . . . . ?
C11 N11 N12 C13 -1.7(5) . . . . ?
C11 N11 C7 N21 139.0(4) . . . . ?
C11 N11 C7 C2 -88.2(5) . . . . ?
C11 C12 C13 N12 -0.4(5) . . . . ?
C21 N21 N22 Re1 177.0(3) . . . . ?
C21 N21 N22 C23 1.8(5) . . . . ?
C21 N21 C7 N11 -133.1(4) . . . . ?
C21 N21 C7 C2 94.5(5) . . . . ?
C21 C22 C23 N22 1.8(5) . . . . ?
C31 P1 C1 C2 127.6(4) . . . . ?
C31 P1 C1 C6 -53.4(4) . . . . ?
C31 P1 C41 C42 -172.2(3) . . . . ?
C31 P1 C41 C46 10.8(4) . . . . ?
C31 C32 C33 C34 -1.3(7) . . . . ?
C32 C31 C36 C35 0.7(6) . . . . ?
C32 C33 C34 C35 1.0(7) . . . . ?
C32 C33 C34 C37 -177.8(4) . . . . ?
C33 C34 C35 C36 0.1(7) . . . . ?
C34 C35 C36 C31 -1.0(7) . . . . ?
C36 C31 C32 C33 0.4(6) . . . . ?
C37 C34 C35 C36 178.9(4) . . . . ?
C41 P1 C1 C2 -123.1(4) . . . . ?
C41 P1 C1 C6 56.0(4) . . . . ?
C41 P1 C31 C32 51.7(4) . . . . ?
C41 P1 C31 C36 -137.9(4) . . . . ?
C41 C42 C43 C44 -0.3(7) . . . . ?
C42 C41 C46 C45 0.4(6) . . . . ?
C42 C43 C44 C45 0.0(7) . . . . ?
C42 C43 C44 C47 -179.5(4) . . . . ?
C43 C44 C45 C46 0.5(6) . . . . ?
C44 C45 C46 C41 -0.7(7) . . . . ?
C46 C41 C42 C43 0.1(6) . . . . ?
C47 C44 C45 C46 -180.0(4) . . . . ?
O3 S1 C14 F1 61.6(4) . . . . ?
O3 S1 C14 F2 -178.8(3) . . . . ?
O3 S1 C14 F3 -58.5(4) . . . . ?
O4 S1 C14 F1 -59.0(4) . . . . ?
O4 S1 C14 F2 60.7(4) . . . . ?
O4 S1 C14 F3 -179.1(3) . . . . ?
O5 S1 C14 F1 -177.8(4) . . . . ?
O5 S1 C14 F2 -58.2(4) . . . . ?
O5 S1 C14 F3 62.1(4) . . . . ?

_olex2_submission_original_sample_id gard25u
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.039
_oxdiff_exptl_absorpt_empirical_full_min 0.636
####################################################################### 
# 
# 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_2-Mn_gard25k
_database_code_depnum_ccdc_archive 'CCDC 2371550'
loop_
_audit_author_name
_audit_author_address
'James Gardinier'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H25 Mn N4 O3 P, C F3 O3 S'
_chemical_formula_sum            'C31 H25 F3 Mn N4 O6 P S'
_chemical_formula_weight         724.52

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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.99461(14)
_cell_length_b                   14.01447(15)
_cell_length_c                   19.1860(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.0115(11)
_cell_angle_gamma                90
_cell_volume                     3207.40(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    13074
_cell_measurement_theta_max      70.5360
_cell_measurement_theta_min      3.8740

_exptl_crystal_description       irregular
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.139
_exptl_absorpt_coefficient_mu    5.021
_shelx_estimated_absorpt_T_min   0.233
_shelx_estimated_absorpt_T_max   0.542
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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   ?
_diffrn_ambient_temperature      100.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Supernova (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_source_current           0.80
_diffrn_measurement_device_type  'Oxford Diffraction Supernova, Dual Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support 'MiTeGen Dual Thickness MicroMount'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryojet Controller'
_diffrn_detector                 'CCD Plate'
_diffrn_detector_type            'Oxford Diffraction Atlas'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_reflns_number            29938
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.705
_diffrn_reflns_theta_max         70.610
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6088
_reflns_number_gt                5662
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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 Ternary CH refined with riding coordinates:
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.4013P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6088
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.01354(2) 0.21589(2) 0.43267(2) 0.01444(8) Uani 1 1 d . . . . .
P1 P 0.20189(3) 0.17319(3) 0.43381(2) 0.01642(10) Uani 1 1 d . . . . .
O1 O -0.06545(11) 0.05759(8) 0.33866(6) 0.0244(3) Uani 1 1 d . . . . .
O2 O -0.02353(11) 0.08566(9) 0.54950(7) 0.0254(3) Uani 1 1 d . . . . .
O3 O -0.22641(11) 0.27381(10) 0.41641(8) 0.0315(3) Uani 1 1 d . . . . .
N11 N 0.11289(11) 0.40947(9) 0.47671(7) 0.0171(3) Uani 1 1 d . . . . .
N12 N 0.06131(11) 0.32929(9) 0.49714(7) 0.0169(3) Uani 1 1 d . . . . .
N21 N 0.10313(11) 0.38121(9) 0.35231(7) 0.0170(3) Uani 1 1 d . . . . .
N22 N 0.04232(11) 0.29932(9) 0.34905(7) 0.0169(3) Uani 1 1 d . . . . .
C1 C 0.30726(14) 0.26906(12) 0.44298(9) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.41826(14) 0.23922(13) 0.46006(9) 0.0236(4) Uani 1 1 d . . . . .
H2 H 0.432623 0.175113 0.469773 0.028 Uiso 1 1 calc R U . . .
C3 C 0.50698(15) 0.30254(14) 0.46284(10) 0.0257(4) Uani 1 1 d . . . . .
H3 H 0.579931 0.281039 0.474393 0.031 Uiso 1 1 calc R U . . .
C4 C 0.48680(15) 0.39769(13) 0.44842(10) 0.0261(4) Uani 1 1 d . . . . .
H4 H 0.546129 0.440626 0.450084 0.031 Uiso 1 1 calc R U . . .
C5 C 0.37782(15) 0.42919(13) 0.43144(9) 0.0235(4) Uani 1 1 d . . . . .
H5 H 0.364639 0.493473 0.421779 0.028 Uiso 1 1 calc R U . . .
C6 C 0.28750(14) 0.36596(12) 0.42861(8) 0.0179(3) Uani 1 1 d . . . . .
C7 C 0.17302(13) 0.41297(11) 0.41468(8) 0.0176(3) Uani 1 1 d . . . . .
H7 H 0.187942 0.480696 0.406956 0.021 Uiso 1 1 calc R U . . .
C8 C -0.03108(13) 0.11822(11) 0.37495(9) 0.0179(3) Uani 1 1 d . . . . .
C9 C -0.00793(13) 0.13801(11) 0.50559(9) 0.0188(3) Uani 1 1 d . . . . .
C10 C -0.13424(14) 0.25363(12) 0.42489(9) 0.0205(3) Uani 1 1 d . . . . .
C11 C 0.04141(14) 0.34549(12) 0.56323(9) 0.0213(3) Uani 1 1 d . . . . .
H11 H 0.005038 0.303003 0.590434 0.026 Uiso 1 1 calc R U . . .
C12 C 0.08234(15) 0.43459(13) 0.58621(9) 0.0230(4) Uani 1 1 d . . . . .
H12 H 0.079162 0.461814 0.630164 0.028 Uiso 1 1 calc R U . . .
C13 C 0.12831(14) 0.47349(12) 0.53001(9) 0.0215(4) Uani 1 1 d . . . . .
H13 H 0.163399 0.532545 0.528709 0.026 Uiso 1 1 calc R U . . .
C21 C 0.00115(14) 0.29068(12) 0.28171(9) 0.0201(3) Uani 1 1 d . . . . .
H21 H -0.044733 0.241033 0.263846 0.024 Uiso 1 1 calc R U . . .
C22 C 0.03636(15) 0.36618(12) 0.24197(9) 0.0222(4) Uani 1 1 d . . . . .
H22 H 0.019416 0.376132 0.194108 0.027 Uiso 1 1 calc R U . . .
C23 C 0.10119(14) 0.42256(12) 0.28838(9) 0.0206(3) Uani 1 1 d . . . . .
H23 H 0.137171 0.478760 0.277940 0.025 Uiso 1 1 calc R U . . .
C31 C 0.23649(14) 0.11852(12) 0.35261(9) 0.0208(3) Uani 1 1 d . . . . .
C32 C 0.29361(15) 0.17045(13) 0.30527(9) 0.0250(4) Uani 1 1 d . . . . .
H32 H 0.311904 0.234018 0.314458 0.030 Uiso 1 1 calc R U . . .
C33 C 0.32305(16) 0.12773(15) 0.24481(10) 0.0306(4) Uani 1 1 d . . . . .
H33 H 0.360068 0.163394 0.213453 0.037 Uiso 1 1 calc R U . . .
C34 C 0.29831(15) 0.03250(15) 0.23009(10) 0.0300(4) Uani 1 1 d . . . . .
C35 C 0.23653(16) -0.01733(13) 0.27507(10) 0.0287(4) Uani 1 1 d . . . . .
H35 H 0.216094 -0.080181 0.264765 0.034 Uiso 1 1 calc R U . . .
C36 C 0.20446(15) 0.02510(13) 0.33549(10) 0.0251(4) Uani 1 1 d . . . . .
H36 H 0.161500 -0.009022 0.364535 0.030 Uiso 1 1 calc R U . . .
C37 C 0.34245(18) -0.01544(18) 0.16862(12) 0.0413(5) Uani 1 1 d . . . . .
H37A H 0.417210 -0.037979 0.182014 0.062 Uiso 1 1 calc R U . . .
H37B H 0.343353 0.029365 0.130832 0.062 Uiso 1 1 calc R U . . .
H37C H 0.295026 -0.068365 0.153696 0.062 Uiso 1 1 calc R U . . .
C41 C 0.25517(14) 0.09515(12) 0.50558(9) 0.0220(4) Uani 1 1 d . . . . .
C42 C 0.30374(16) 0.00612(14) 0.49812(11) 0.0306(4) Uani 1 1 d . . . . .
H42 H 0.309683 -0.018601 0.453683 0.037 Uiso 1 1 calc R U . . .
C43 C 0.34346(17) -0.04591(15) 0.55747(13) 0.0388(5) Uani 1 1 d . . . . .
H43 H 0.374553 -0.105847 0.551823 0.047 Uiso 1 1 calc R U . . .
C44 C 0.33813(16) -0.01140(17) 0.62410(12) 0.0388(5) Uani 1 1 d . . . . .
C45 C 0.29016(17) 0.07847(17) 0.63134(11) 0.0368(5) Uani 1 1 d . . . . .
H45 H 0.286020 0.103544 0.675873 0.044 Uiso 1 1 calc R U . . .
C46 C 0.24881(16) 0.13054(15) 0.57313(10) 0.0293(4) Uani 1 1 d . . . . .
H46 H 0.216338 0.189874 0.578987 0.035 Uiso 1 1 calc R U . . .
C47 C 0.3816(2) -0.0686(2) 0.68773(15) 0.0611(8) Uani 1 1 d . . . . .
H47A H 0.432210 -0.030051 0.717931 0.092 Uiso 1 1 calc R U . . .
H47B H 0.420455 -0.123904 0.673308 0.092 Uiso 1 1 calc R U . . .
H47C H 0.319967 -0.088179 0.712467 0.092 Uiso 1 1 calc R U . . .
S3 S 0.22939(3) 0.69498(3) 0.36929(2) 0.02129(10) Uani 1 1 d . . . . .
F1 F 0.36596(11) 0.77212(9) 0.28659(6) 0.0382(3) Uani 1 1 d . . . . .
F2 F 0.44259(10) 0.66615(9) 0.35723(7) 0.0424(3) Uani 1 1 d . . . . .
F3 F 0.40527(10) 0.80582(8) 0.39561(7) 0.0375(3) Uani 1 1 d . . . . .
O4 O 0.16496(11) 0.78104(9) 0.36985(8) 0.0319(3) Uani 1 1 d . . . . .
O5 O 0.19608(13) 0.63206(11) 0.31138(8) 0.0409(4) Uani 1 1 d . . . . .
O6 O 0.25081(11) 0.64699(10) 0.43601(7) 0.0305(3) Uani 1 1 d . . . . .
C14 C 0.36805(16) 0.73689(13) 0.35138(10) 0.0274(4) 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
Mn1 C8 1.8062(17) . ?
Mn1 C9 1.8139(18) . ?
Mn1 C10 1.8409(18) . ?
Mn1 N22 2.0437(14) . ?
Mn1 N12 2.0580(14) . ?
Mn1 P1 2.3350(5) . ?
P1 C41 1.8211(17) . ?
P1 C31 1.8226(18) . ?
P1 C1 1.8403(17) . ?
O1 C8 1.147(2) . ?
O2 C9 1.147(2) . ?
O3 C10 1.136(2) . ?
N11 C13 1.358(2) . ?
N11 N12 1.3601(19) . ?
N11 C7 1.456(2) . ?
N12 C11 1.334(2) . ?
N21 C23 1.354(2) . ?
N21 N22 1.3577(19) . ?
N21 C7 1.457(2) . ?
N22 C21 1.339(2) . ?
C1 C6 1.401(2) . ?
C1 C2 1.401(2) . ?
C2 C3 1.382(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.521(2) . ?
C7 H7 0.9800 . ?
C11 C12 1.396(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C21 C22 1.395(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.370(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C31 C36 1.394(2) . ?
C31 C32 1.398(3) . ?
C32 C33 1.384(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.390(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.384(3) . ?
C34 C37 1.501(3) . ?
C35 C36 1.392(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.391(3) . ?
C41 C46 1.397(3) . ?
C42 C43 1.393(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.375(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.398(3) . ?
C44 C47 1.507(3) . ?
C45 C46 1.382(3) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
S3 O4 1.4330(13) . ?
S3 O5 1.4417(14) . ?
S3 O6 1.4451(13) . ?
S3 C14 1.830(2) . ?
F1 C14 1.335(2) . ?
F2 C14 1.332(2) . ?
F3 C14 1.332(2) . ?

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
C8 Mn1 C9 87.71(7) . . ?
C8 Mn1 C10 86.96(7) . . ?
C9 Mn1 C10 91.27(7) . . ?
C8 Mn1 N22 90.90(6) . . ?
C9 Mn1 N22 177.53(7) . . ?
C10 Mn1 N22 90.70(7) . . ?
C8 Mn1 N12 178.56(6) . . ?
C9 Mn1 N12 93.10(6) . . ?
C10 Mn1 N12 91.84(6) . . ?
N22 Mn1 N12 88.32(5) . . ?
C8 Mn1 P1 92.05(5) . . ?
C9 Mn1 P1 93.10(5) . . ?
C10 Mn1 P1 175.48(5) . . ?
N22 Mn1 P1 84.90(4) . . ?
N12 Mn1 P1 89.09(4) . . ?
C41 P1 C31 107.49(8) . . ?
C41 P1 C1 100.55(8) . . ?
C31 P1 C1 99.96(8) . . ?
C41 P1 Mn1 115.06(6) . . ?
C31 P1 Mn1 113.98(5) . . ?
C1 P1 Mn1 117.90(6) . . ?
C13 N11 N12 111.03(14) . . ?
C13 N11 C7 123.58(14) . . ?
N12 N11 C7 122.88(13) . . ?
C11 N12 N11 105.39(13) . . ?
C11 N12 Mn1 129.52(11) . . ?
N11 N12 Mn1 124.83(10) . . ?
C23 N21 N22 111.21(13) . . ?
C23 N21 C7 124.53(14) . . ?
N22 N21 C7 123.79(13) . . ?
C21 N22 N21 105.24(13) . . ?
C21 N22 Mn1 129.05(11) . . ?
N21 N22 Mn1 125.56(10) . . ?
C6 C1 C2 118.18(15) . . ?
C6 C1 P1 126.05(13) . . ?
C2 C1 P1 115.51(13) . . ?
C3 C2 C1 121.75(17) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 119.67(17) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.80(17) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 121.06(16) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.53(15) . . ?
C5 C6 C7 114.49(14) . . ?
C1 C6 C7 125.83(15) . . ?
N11 C7 N21 111.68(13) . . ?
N11 C7 C6 110.92(13) . . ?
N21 C7 C6 116.31(13) . . ?
N11 C7 H7 105.7 . . ?
N21 C7 H7 105.7 . . ?
C6 C7 H7 105.7 . . ?
O1 C8 Mn1 176.21(15) . . ?
O2 C9 Mn1 176.82(15) . . ?
O3 C10 Mn1 175.83(16) . . ?
N12 C11 C12 111.12(16) . . ?
N12 C11 H11 124.4 . . ?
C12 C11 H11 124.4 . . ?
C13 C12 C11 105.29(15) . . ?
C13 C12 H12 127.4 . . ?
C11 C12 H12 127.4 . . ?
N11 C13 C12 107.12(15) . . ?
N11 C13 H13 126.4 . . ?
C12 C13 H13 126.4 . . ?
N22 C21 C22 110.88(15) . . ?
N22 C21 H21 124.6 . . ?
C22 C21 H21 124.6 . . ?
C23 C22 C21 105.42(15) . . ?
C23 C22 H22 127.3 . . ?
C21 C22 H22 127.3 . . ?
N21 C23 C22 107.25(14) . . ?
N21 C23 H23 126.4 . . ?
C22 C23 H23 126.4 . . ?
C36 C31 C32 118.53(16) . . ?
C36 C31 P1 120.96(14) . . ?
C32 C31 P1 120.50(13) . . ?
C33 C32 C31 120.33(17) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 121.20(18) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C35 C34 C33 118.34(17) . . ?
C35 C34 C37 121.33(19) . . ?
C33 C34 C37 120.3(2) . . ?
C34 C35 C36 121.08(17) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 120.26(18) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 118.56(17) . . ?
C42 C41 P1 125.35(15) . . ?
C46 C41 P1 116.06(13) . . ?
C41 C42 C43 119.8(2) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 122.0(2) . . ?
C44 C43 H43 119.0 . . ?
C42 C43 H43 119.0 . . ?
C43 C44 C45 117.98(18) . . ?
C43 C44 C47 121.4(2) . . ?
C45 C44 C47 120.7(2) . . ?
C46 C45 C44 120.8(2) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C41 120.82(19) . . ?
C45 C46 H46 119.6 . . ?
C41 C46 H46 119.6 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 S3 O5 114.48(9) . . ?
O4 S3 O6 115.53(9) . . ?
O5 S3 O6 114.03(9) . . ?
O4 S3 C14 103.46(8) . . ?
O5 S3 C14 103.62(9) . . ?
O6 S3 C14 103.59(8) . . ?
F3 C14 F2 108.00(15) . . ?
F3 C14 F1 107.30(15) . . ?
F2 C14 F1 107.50(16) . . ?
F3 C14 S3 111.33(13) . . ?
F2 C14 S3 111.14(13) . . ?
F1 C14 S3 111.38(13) . . ?

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
C13 N11 N12 C11 2.01(17) . . . . ?
C7 N11 N12 C11 164.59(14) . . . . ?
C13 N11 N12 Mn1 176.70(10) . . . . ?
C7 N11 N12 Mn1 -20.72(19) . . . . ?
C23 N21 N22 C21 -0.63(18) . . . . ?
C7 N21 N22 C21 -173.05(15) . . . . ?
C23 N21 N22 Mn1 -176.50(11) . . . . ?
C7 N21 N22 Mn1 11.1(2) . . . . ?
C41 P1 C1 C6 -146.38(15) . . . . ?
C31 P1 C1 C6 103.55(16) . . . . ?
Mn1 P1 C1 C6 -20.51(17) . . . . ?
C41 P1 C1 C2 39.52(15) . . . . ?
C31 P1 C1 C2 -70.55(14) . . . . ?
Mn1 P1 C1 C2 165.39(11) . . . . ?
C6 C1 C2 C3 -0.1(3) . . . . ?
P1 C1 C2 C3 174.51(14) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C3 C4 C5 C6 0.0(3) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
C4 C5 C6 C7 175.59(16) . . . . ?
C2 C1 C6 C5 0.2(2) . . . . ?
P1 C1 C6 C5 -173.74(13) . . . . ?
C2 C1 C6 C7 -175.02(16) . . . . ?
P1 C1 C6 C7 11.0(2) . . . . ?
C13 N11 C7 N21 -145.37(15) . . . . ?
N12 N11 C7 N21 54.23(19) . . . . ?
C13 N11 C7 C6 83.13(18) . . . . ?
N12 N11 C7 C6 -77.27(17) . . . . ?
C23 N21 C7 N11 139.53(16) . . . . ?
N22 N21 C7 N11 -49.1(2) . . . . ?
C23 N21 C7 C6 -91.76(19) . . . . ?
N22 N21 C7 C6 79.65(19) . . . . ?
C5 C6 C7 N11 -109.98(16) . . . . ?
C1 C6 C7 N11 65.5(2) . . . . ?
C5 C6 C7 N21 120.95(16) . . . . ?
C1 C6 C7 N21 -63.6(2) . . . . ?
N11 N12 C11 C12 -1.52(18) . . . . ?
Mn1 N12 C11 C12 -175.87(11) . . . . ?
N12 C11 C12 C13 0.50(19) . . . . ?
N12 N11 C13 C12 -1.74(18) . . . . ?
C7 N11 C13 C12 -164.17(14) . . . . ?
C11 C12 C13 N11 0.74(18) . . . . ?
N21 N22 C21 C22 0.58(19) . . . . ?
Mn1 N22 C21 C22 176.26(12) . . . . ?
N22 C21 C22 C23 -0.3(2) . . . . ?
N22 N21 C23 C22 0.43(19) . . . . ?
C7 N21 C23 C22 172.78(15) . . . . ?
C21 C22 C23 N21 -0.06(19) . . . . ?
C41 P1 C31 C36 54.56(16) . . . . ?
C1 P1 C31 C36 159.05(14) . . . . ?
Mn1 P1 C31 C36 -74.21(15) . . . . ?
C41 P1 C31 C32 -126.98(14) . . . . ?
C1 P1 C31 C32 -22.49(15) . . . . ?
Mn1 P1 C31 C32 104.25(14) . . . . ?
C36 C31 C32 C33 -3.7(3) . . . . ?
P1 C31 C32 C33 177.82(14) . . . . ?
C31 C32 C33 C34 -0.9(3) . . . . ?
C32 C33 C34 C35 4.3(3) . . . . ?
C32 C33 C34 C37 -172.95(18) . . . . ?
C33 C34 C35 C36 -3.1(3) . . . . ?
C37 C34 C35 C36 174.12(18) . . . . ?
C34 C35 C36 C31 -1.5(3) . . . . ?
C32 C31 C36 C35 4.8(3) . . . . ?
P1 C31 C36 C35 -176.66(14) . . . . ?
C31 P1 C41 C42 -5.45(18) . . . . ?
C1 P1 C41 C42 -109.53(16) . . . . ?
Mn1 P1 C41 C42 122.71(15) . . . . ?
C31 P1 C41 C46 172.52(14) . . . . ?
C1 P1 C41 C46 68.44(15) . . . . ?
Mn1 P1 C41 C46 -59.33(15) . . . . ?
C46 C41 C42 C43 0.7(3) . . . . ?
P1 C41 C42 C43 178.65(15) . . . . ?
C41 C42 C43 C44 -1.1(3) . . . . ?
C42 C43 C44 C45 0.6(3) . . . . ?
C42 C43 C44 C47 -179.9(2) . . . . ?
C43 C44 C45 C46 0.4(3) . . . . ?
C47 C44 C45 C46 -179.1(2) . . . . ?
C44 C45 C46 C41 -0.8(3) . . . . ?
C42 C41 C46 C45 0.2(3) . . . . ?
P1 C41 C46 C45 -177.90(15) . . . . ?
O4 S3 C14 F3 52.22(15) . . . . ?
O5 S3 C14 F3 171.99(13) . . . . ?
O6 S3 C14 F3 -68.69(14) . . . . ?
O4 S3 C14 F2 172.66(13) . . . . ?
O5 S3 C14 F2 -67.57(15) . . . . ?
O6 S3 C14 F2 51.74(15) . . . . ?
O4 S3 C14 F1 -67.49(15) . . . . ?
O5 S3 C14 F1 52.27(15) . . . . ?
O6 S3 C14 F1 171.59(13) . . . . ?

_refine_diff_density_max         0.409
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.050


####################################################################### 
# 
# 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_4_CH3CN_H2O_gard25q
_database_code_depnum_ccdc_archive 'CCDC 2371553'
loop_
_audit_author_name
_audit_author_address
'James Gardinier'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_audit_creation_date             2024-03-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/1
loop_
_audit_author_email
james.gardinier@marquette.edu
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C28 H25 F3 Mn0.5 N4 O4 P S'
_chemical_formula_sum            'C28 H25 F3 Mn0.50 N4 O4 P S'
_chemical_formula_weight         629.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         C28H25N4F3O3PMnS
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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'
S S 0.3331 0.5567 '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                   9.3815(3)
_cell_length_b                   12.9857(4)
_cell_length_c                   13.0750(5)
_cell_angle_alpha                64.443(3)
_cell_angle_beta                 85.597(3)
_cell_angle_gamma                88.991(3)
_cell_volume                     1432.55(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11411
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      70.5590
_cell_measurement_theta_min      3.9770
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.605
_exptl_absorpt_coefficient_mu    3.781
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             647
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 8 0.0236
0 -1 -8 0.0366
0 -8 -2 0.0487
0 8 2 0.0467
6 0 1 0.0549
-6 0 -1 0.0879

_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.06
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
-0.0000 1.0000 8.0000 -0.6874 0.7228 0.0410
0.0000 -1.0000 -8.0000 0.6874 -0.7228 -0.0410
0.0000 -8.0000 -2.0000 -0.7147 -0.5525 -0.3491
-0.0000 8.0000 2.0000 0.7147 0.5525 0.3491
6.0000 0.0000 1.0000 -0.2875 -0.2521 0.9099
-6.0000 -0.0000 -1.0000 0.2875 0.2521 -0.9099

_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26350
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        70.537
_diffrn_reflns_theta_max         70.537
_diffrn_reflns_theta_min         3.758
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -67.00   1.00    1.98    --  -42.46-134.00 106.00   48
  2  ω    -67.00  32.00   1.00    1.98    --  -42.46  37.00 120.00   99
  3  ω   -117.00 -18.00   1.00    1.98    --  -42.46 -37.00 -60.00   99
  4  ω     18.00 117.00   1.00    1.98    --   42.46  37.00-180.00   99
  5  ω     29.00 104.00   1.00    1.98    --   42.46-135.00 -73.00   75
  6  ω     94.00 173.00   1.00    7.91    --  100.00 125.00 -90.00   79
  7  ω     17.00 110.00   1.00    7.91    --  100.00 -94.00 120.00   93
  8  ω     27.00 118.00   1.00    7.91    --  100.00-125.00  90.00   91
  9  ω     17.00 110.00   1.00    7.91    --  100.00 -94.00 -60.00   93
 10  ω     74.00 173.00   1.00    7.91    --  100.00  45.00  90.00   99
 11  ω     71.00 172.00   1.00    7.91    --  100.00  61.00  30.00  101
 12  ω     28.00 129.00   1.00    7.91    --  100.00 -61.00 -30.00  101
 13  ω     27.00 118.00   1.00    7.91    --  100.00-125.00-120.00   91
 14  ω     71.00 172.00   1.00    7.91    --  100.00  61.00   0.00  101
 15  ω     24.00 133.00   1.00    7.91    --  100.00 -77.00-180.00  109
 16  ω     71.00 172.00   1.00    7.91    --  100.00  61.00 -30.00  101
 17  ω     67.00 176.00   1.00    7.91    --  100.00  77.00-120.00  109
 18  ω   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00-150.00  109
 19  ω   -115.00 -14.00   1.00    1.98    --  -42.46 -57.00  60.00  101
 20  ω   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00  30.00  109
 21  ω   -119.00 -10.00   1.00    1.98    --  -42.46 -77.00 -60.00  109
 22  ω     23.00  98.00   1.00    1.98    --   42.46-125.00  30.00   75
 23  ω     71.00 172.00   1.00    7.91    --  100.00  61.00 120.00  101
 24  ω     67.00 169.00   1.00    7.91    --  100.00  77.00  30.00  102
 25  ω     72.00 176.00   1.00    7.91    --  100.00  30.00-180.00  104
 26  ω     71.00 172.00   1.00    7.91    --  100.00  61.00  90.00  101
 27  ω     71.00 172.00   1.00    7.91    --  100.00  61.00-180.00  101
 28  ω     67.00 176.00   1.00    7.91    --  100.00  77.00 -90.00  109
 29  ω     71.00 172.00   1.00    7.91    --  100.00  61.00-150.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0312100000
_diffrn_orient_matrix_UB_12      0.1143865000
_diffrn_orient_matrix_UB_13      -0.1002182000
_diffrn_orient_matrix_UB_21      -0.0560803000
_diffrn_orient_matrix_UB_22      0.0479741000
_diffrn_orient_matrix_UB_23      0.0843475000
_diffrn_orient_matrix_UB_31      0.1517067000
_diffrn_orient_matrix_UB_32      0.0437272000
_diffrn_orient_matrix_UB_33      -0.0003430000
_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                5009
_reflns_number_total             5431
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.042
_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)+(0.0438P)²+0.5294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0815
_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 Ternary CH refined with riding coordinates:
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.500000 0.500000 0.500000 0.01565(9) Uani 1 2 d S . P . .
S2 S 0.63312(4) 0.24050(3) 0.62568(3) 0.01965(10) Uani 1 1 d . . . . .
P1 P 0.44702(4) 0.53750(3) 0.74640(3) 0.01667(10) Uani 1 1 d . . . . .
F1 F 0.53723(16) 0.14233(11) 0.84104(10) 0.0508(4) Uani 1 1 d . . . . .
F2 F 0.76191(16) 0.18254(12) 0.81359(11) 0.0512(3) Uani 1 1 d . . . . .
F3 F 0.68121(15) 0.04115(10) 0.78988(11) 0.0450(3) Uani 1 1 d . . . . .
O1 O 0.42385(12) 0.54757(9) 0.62993(9) 0.0177(2) Uani 1 1 d . . . . .
O2 O 0.59473(13) 0.34793(10) 0.62982(10) 0.0240(3) Uani 1 1 d . . . . .
O3 O 0.51895(13) 0.18768(10) 0.59751(11) 0.0277(3) Uani 1 1 d . . . . .
O4 O 0.77093(13) 0.24012(12) 0.57082(12) 0.0310(3) Uani 1 1 d . . . . .
N11 N 0.77742(14) 0.67198(11) 0.49495(12) 0.0186(3) Uani 1 1 d . . . . .
N12 N 0.72593(15) 0.58800(11) 0.47062(12) 0.0193(3) Uani 1 1 d . . . . .
N21 N 0.73960(15) 0.79522(12) 0.58861(12) 0.0201(3) Uani 1 1 d . . . . .
N22 N 0.86688(16) 0.81756(14) 0.61879(16) 0.0321(4) Uani 1 1 d . . . . .
C1 C 0.63205(17) 0.51173(14) 0.77725(14) 0.0185(3) Uani 1 1 d . . . . .
C2 C 0.74009(17) 0.58412(14) 0.70193(14) 0.0190(3) Uani 1 1 d . . . . .
C3 C 0.88259(18) 0.55861(15) 0.72539(15) 0.0220(3) Uani 1 1 d . . . . .
H3 H 0.955248 0.605723 0.675694 0.026 Uiso 1 1 calc R U . . .
C4 C 0.91689(19) 0.46360(15) 0.82219(15) 0.0258(4) Uani 1 1 d . . . . .
H4 H 1.012191 0.447713 0.836978 0.031 Uiso 1 1 calc R U . . .
C5 C 0.8101(2) 0.39252(15) 0.89665(15) 0.0262(4) Uani 1 1 d . . . . .
H5 H 0.833417 0.329193 0.961612 0.031 Uiso 1 1 calc R U . . .
C6 C 0.66834(19) 0.41606(15) 0.87407(14) 0.0231(3) Uani 1 1 d . . . . .
H6 H 0.596569 0.367778 0.923766 0.028 Uiso 1 1 calc R U . . .
C7 C 0.70555(17) 0.68547(13) 0.59193(14) 0.0180(3) Uani 1 1 d . . . . .
H7 H 0.602326 0.682949 0.585832 0.022 Uiso 1 1 calc R U . . .
C11 C 0.91222(18) 0.70435(15) 0.44803(15) 0.0232(3) Uani 1 1 d . . . . .
H11 H 0.968967 0.758533 0.455195 0.028 Uiso 1 1 calc R U . . .
C12 C 0.94954(19) 0.64262(17) 0.38811(16) 0.0279(4) Uani 1 1 d . . . . .
H12 H 1.035064 0.646967 0.345360 0.033 Uiso 1 1 calc R U . . .
C13 C 0.83145(18) 0.57165(16) 0.40503(16) 0.0254(4) Uani 1 1 d . . . . .
H13 H 0.826870 0.519303 0.374287 0.030 Uiso 1 1 calc R U . . .
C14 C 0.6546(2) 0.14718(16) 0.77568(16) 0.0305(4) Uani 1 1 d . . . . .
C21 C 0.6512(2) 0.88541(15) 0.55892(15) 0.0257(4) Uani 1 1 d . . . . .
H21 H 0.559390 0.888694 0.535592 0.031 Uiso 1 1 calc R U . . .
C22 C 0.7221(2) 0.97038(15) 0.56965(16) 0.0284(4) Uani 1 1 d . . . . .
H22 H 0.689532 1.042908 0.555880 0.034 Uiso 1 1 calc R U . . .
C23 C 0.8544(2) 0.92438(16) 0.60589(17) 0.0295(4) Uani 1 1 d . . . . .
H23 H 0.926226 0.964245 0.619564 0.035 Uiso 1 1 calc R U . . .
C31 C 0.39886(17) 0.66670(14) 0.75745(13) 0.0194(3) Uani 1 1 d . . . . .
C32 C 0.28297(19) 0.72690(16) 0.70062(15) 0.0256(4) Uani 1 1 d . . . . .
H32 H 0.232611 0.699923 0.658326 0.031 Uiso 1 1 calc R U . . .
C33 C 0.2429(2) 0.82726(16) 0.70731(17) 0.0306(4) Uani 1 1 d . . . . .
H33 H 0.164943 0.866721 0.669565 0.037 Uiso 1 1 calc R U . . .
C34 C 0.3167(2) 0.87022(15) 0.76926(16) 0.0287(4) Uani 1 1 d . . . . .
C35 C 0.4320(2) 0.80924(16) 0.82582(16) 0.0289(4) Uani 1 1 d . . . . .
H35 H 0.482285 0.836351 0.868050 0.035 Uiso 1 1 calc R U . . .
C36 C 0.47333(19) 0.70844(15) 0.82027(14) 0.0236(3) Uani 1 1 d . . . . .
H36 H 0.550826 0.668722 0.858550 0.028 Uiso 1 1 calc R U . . .
C37 C 0.2760(2) 0.98228(17) 0.7714(2) 0.0426(5) Uani 1 1 d . . . . .
H37A H 0.281006 0.976004 0.846925 0.064 Uiso 1 1 calc R U . . .
H37B H 0.180355 1.000701 0.748901 0.064 Uiso 1 1 calc R U . . .
H37C H 0.340835 1.041420 0.719712 0.064 Uiso 1 1 calc R U . . .
C41 C 0.33950(17) 0.42334(14) 0.85341(14) 0.0204(3) Uani 1 1 d . . . . .
C42 C 0.3191(2) 0.32480(15) 0.83859(15) 0.0266(4) Uani 1 1 d . . . . .
H42 H 0.364045 0.317949 0.775954 0.032 Uiso 1 1 calc R U . . .
C43 C 0.2319(2) 0.23701(16) 0.91719(17) 0.0323(4) Uani 1 1 d . . . . .
H43 H 0.218612 0.171634 0.906476 0.039 Uiso 1 1 calc R U . . .
C44 C 0.16354(19) 0.24484(16) 1.01219(15) 0.0294(4) Uani 1 1 d . . . . .
C45 C 0.18593(19) 0.34270(17) 1.02709(15) 0.0286(4) Uani 1 1 d . . . . .
H45 H 0.142383 0.348717 1.090585 0.034 Uiso 1 1 calc R U . . .
C46 C 0.27230(19) 0.43173(16) 0.94871(14) 0.0249(4) Uani 1 1 d . . . . .
H46 H 0.285496 0.497034 0.959575 0.030 Uiso 1 1 calc R U . . .
C47 C 0.0652(2) 0.15024(19) 1.09451(19) 0.0425(5) Uani 1 1 d . . . . .
H47A H 0.120910 0.087384 1.141911 0.064 Uiso 1 1 calc R U . . .
H47B H 0.004892 0.125415 1.053087 0.064 Uiso 1 1 calc R U . . .
H47C H 0.007126 0.177580 1.141026 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
Mn1 O1 2.1169(10) 2_666 ?
Mn1 O1 2.1169(10) . ?
Mn1 O2 2.2019(11) . ?
Mn1 O2 2.2019(11) 2_666 ?
Mn1 N12 2.3510(14) 2_666 ?
Mn1 N12 2.3511(14) . ?
S2 O2 1.4571(12) . ?
S2 O3 1.4344(13) . ?
S2 O4 1.4305(13) . ?
S2 C14 1.8322(19) . ?
P1 O1 1.5038(11) . ?
P1 C1 1.8051(17) . ?
P1 C31 1.7922(16) . ?
P1 C41 1.7942(17) . ?
F1 C14 1.326(2) . ?
F2 C14 1.326(2) . ?
F3 C14 1.329(2) . ?
N11 N12 1.3658(19) . ?
N11 C7 1.466(2) . ?
N11 C11 1.353(2) . ?
N12 C13 1.334(2) . ?
N21 N22 1.360(2) . ?
N21 C7 1.448(2) . ?
N21 C21 1.354(2) . ?
N22 C23 1.327(2) . ?
C1 C2 1.401(2) . ?
C1 C6 1.399(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.526(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.367(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.396(3) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.361(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.393(3) . ?
C23 H23 0.9300 . ?
C31 C32 1.392(2) . ?
C31 C36 1.394(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.387(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.392(3) . ?
C34 C35 1.390(3) . ?
C34 C37 1.509(2) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(2) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.393(2) . ?
C41 C46 1.399(2) . ?
C42 H42 0.9300 . ?
C42 C43 1.385(3) . ?
C43 H43 0.9300 . ?
C43 C44 1.396(3) . ?
C44 C45 1.388(3) . ?
C44 C47 1.505(3) . ?
C45 H45 0.9300 . ?
C45 C46 1.388(3) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 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
O1 Mn1 O1 180.0 2_666 . ?
O1 Mn1 O2 88.88(4) . . ?
O1 Mn1 O2 91.12(4) 2_666 . ?
O1 Mn1 O2 91.12(4) . 2_666 ?
O1 Mn1 O2 88.88(4) 2_666 2_666 ?
O1 Mn1 N12 85.16(4) . 2_666 ?
O1 Mn1 N12 94.84(4) 2_666 2_666 ?
O1 Mn1 N12 94.84(4) . . ?
O1 Mn1 N12 85.16(4) 2_666 . ?
O2 Mn1 O2 180.0 2_666 . ?
O2 Mn1 N12 86.31(5) . . ?
O2 Mn1 N12 86.31(5) 2_666 2_666 ?
O2 Mn1 N12 93.69(5) . 2_666 ?
O2 Mn1 N12 93.69(5) 2_666 . ?
N12 Mn1 N12 180.0 2_666 . ?
O2 S2 C14 101.79(8) . . ?
O3 S2 O2 113.85(7) . . ?
O3 S2 C14 104.12(9) . . ?
O4 S2 O2 115.16(8) . . ?
O4 S2 O3 115.93(8) . . ?
O4 S2 C14 103.54(9) . . ?
O1 P1 C1 111.55(7) . . ?
O1 P1 C31 110.72(7) . . ?
O1 P1 C41 110.72(7) . . ?
C31 P1 C1 107.21(8) . . ?
C31 P1 C41 107.87(8) . . ?
C41 P1 C1 108.63(8) . . ?
P1 O1 Mn1 145.07(7) . . ?
S2 O2 Mn1 128.94(7) . . ?
N12 N11 C7 116.98(13) . . ?
C11 N11 N12 111.57(13) . . ?
C11 N11 C7 127.96(14) . . ?
N11 N12 Mn1 133.54(10) . . ?
C13 N12 Mn1 121.54(11) . . ?
C13 N12 N11 104.27(13) . . ?
N22 N21 C7 122.31(13) . . ?
C21 N21 N22 112.11(14) . . ?
C21 N21 C7 125.55(14) . . ?
C23 N22 N21 103.47(14) . . ?
C2 C1 P1 120.31(12) . . ?
C6 C1 P1 119.88(13) . . ?
C6 C1 C2 119.74(15) . . ?
C1 C2 C7 121.39(14) . . ?
C3 C2 C1 118.90(15) . . ?
C3 C2 C7 119.61(15) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.68(16) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.35(16) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.69(16) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.64(17) . . ?
C5 C6 H6 119.7 . . ?
N11 C7 C2 109.24(12) . . ?
N11 C7 H7 107.4 . . ?
N21 C7 N11 111.36(13) . . ?
N21 C7 C2 113.78(13) . . ?
N21 C7 H7 107.4 . . ?
C2 C7 H7 107.4 . . ?
N11 C11 H11 126.4 . . ?
N11 C11 C12 107.26(15) . . ?
C12 C11 H11 126.4 . . ?
C11 C12 H12 127.5 . . ?
C11 C12 C13 105.04(15) . . ?
C13 C12 H12 127.5 . . ?
N12 C13 C12 111.82(15) . . ?
N12 C13 H13 124.1 . . ?
C12 C13 H13 124.1 . . ?
F1 C14 S2 111.78(13) . . ?
F1 C14 F2 108.01(16) . . ?
F1 C14 F3 106.99(17) . . ?
F2 C14 S2 111.41(14) . . ?
F2 C14 F3 108.00(15) . . ?
F3 C14 S2 110.46(13) . . ?
N21 C21 H21 126.5 . . ?
N21 C21 C22 107.08(16) . . ?
C22 C21 H21 126.5 . . ?
C21 C22 H22 127.7 . . ?
C21 C22 C23 104.56(15) . . ?
C23 C22 H22 127.7 . . ?
N22 C23 C22 112.77(16) . . ?
N22 C23 H23 123.6 . . ?
C22 C23 H23 123.6 . . ?
C32 C31 P1 118.27(13) . . ?
C32 C31 C36 119.38(15) . . ?
C36 C31 P1 122.34(13) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.76(17) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 119.3 . . ?
C32 C33 C34 121.46(17) . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C37 120.84(19) . . ?
C35 C34 C33 118.25(16) . . ?
C35 C34 C37 120.88(19) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 C34 121.04(17) . . ?
C36 C35 H35 119.5 . . ?
C31 C36 H36 119.9 . . ?
C35 C36 C31 120.11(17) . . ?
C35 C36 H36 119.9 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 P1 118.50(13) . . ?
C42 C41 C46 119.27(16) . . ?
C46 C41 P1 122.20(13) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 119.97(16) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 119.4 . . ?
C42 C43 C44 121.22(18) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 C47 120.41(19) . . ?
C45 C44 C43 118.43(17) . . ?
C45 C44 C47 121.13(18) . . ?
C44 C45 H45 119.5 . . ?
C44 C45 C46 121.03(16) . . ?
C46 C45 H45 119.5 . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.07(17) . . ?
C45 C46 H46 120.0 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 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 N12 C13 C12 172.57(12) . . . . ?
P1 C1 C2 C3 -176.84(12) . . . . ?
P1 C1 C2 C7 -0.6(2) . . . . ?
P1 C1 C6 C5 177.44(13) . . . . ?
P1 C31 C32 C33 -179.96(14) . . . . ?
P1 C31 C36 C35 179.77(13) . . . . ?
P1 C41 C42 C43 -177.31(15) . . . . ?
P1 C41 C46 C45 177.64(13) . . . . ?
O1 P1 C1 C2 53.06(14) . . . . ?
O1 P1 C1 C6 -123.94(13) . . . . ?
O1 P1 C31 C32 35.77(16) . . . . ?
O1 P1 C31 C36 -144.06(14) . . . . ?
O1 P1 C41 C42 36.56(16) . . . . ?
O1 P1 C41 C46 -141.35(14) . . . . ?
O2 S2 C14 F1 56.89(15) . . . . ?
O2 S2 C14 F2 -64.07(15) . . . . ?
O2 S2 C14 F3 175.90(14) . . . . ?
O3 S2 O2 Mn1 -53.02(12) . . . . ?
O3 S2 C14 F1 -61.69(15) . . . . ?
O3 S2 C14 F2 177.36(13) . . . . ?
O3 S2 C14 F3 57.32(16) . . . . ?
O4 S2 O2 Mn1 84.35(11) . . . . ?
O4 S2 C14 F1 176.69(13) . . . . ?
O4 S2 C14 F2 55.73(15) . . . . ?
O4 S2 C14 F3 -64.30(16) . . . . ?
N11 N12 C13 C12 0.6(2) . . . . ?
N11 C11 C12 C13 -1.3(2) . . . . ?
N12 N11 C7 N21 -162.81(13) . . . . ?
N12 N11 C7 C2 70.68(17) . . . . ?
N12 N11 C11 C12 1.8(2) . . . . ?
N21 N22 C23 C22 0.7(2) . . . . ?
N21 C21 C22 C23 0.4(2) . . . . ?
N22 N21 C7 N11 -76.83(19) . . . . ?
N22 N21 C7 C2 47.1(2) . . . . ?
N22 N21 C21 C22 0.0(2) . . . . ?
C1 P1 O1 Mn1 26.42(14) . . . . ?
C1 P1 C31 C32 157.66(14) . . . . ?
C1 P1 C31 C36 -22.17(16) . . . . ?
C1 P1 C41 C42 -86.25(15) . . . . ?
C1 P1 C41 C46 95.84(15) . . . . ?
C1 C2 C3 C4 -0.5(2) . . . . ?
C1 C2 C7 N11 -120.24(15) . . . . ?
C1 C2 C7 N21 114.64(16) . . . . ?
C2 C1 C6 C5 0.4(2) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C3 C2 C7 N11 56.02(18) . . . . ?
C3 C2 C7 N21 -69.10(19) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C4 C5 C6 C1 -0.7(3) . . . . ?
C6 C1 C2 C3 0.2(2) . . . . ?
C6 C1 C2 C7 176.45(14) . . . . ?
C7 N11 N12 Mn1 27.3(2) . . . . ?
C7 N11 N12 C13 -162.16(14) . . . . ?
C7 N11 C11 C12 159.83(16) . . . . ?
C7 N21 N22 C23 -178.98(16) . . . . ?
C7 N21 C21 C22 178.49(16) . . . . ?
C7 C2 C3 C4 -176.85(15) . . . . ?
C11 N11 N12 Mn1 -172.03(12) . . . . ?
C11 N11 N12 C13 -1.52(18) . . . . ?
C11 N11 C7 N21 40.2(2) . . . . ?
C11 N11 C7 C2 -86.30(19) . . . . ?
C11 C12 C13 N12 0.4(2) . . . . ?
C14 S2 O2 Mn1 -164.41(10) . . . . ?
C21 N21 N22 C23 -0.5(2) . . . . ?
C21 N21 C7 N11 104.87(18) . . . . ?
C21 N21 C7 C2 -131.15(17) . . . . ?
C21 C22 C23 N22 -0.7(2) . . . . ?
C31 P1 O1 Mn1 145.73(12) . . . . ?
C31 P1 C1 C2 -68.30(14) . . . . ?
C31 P1 C1 C6 114.69(13) . . . . ?
C31 P1 C41 C42 157.85(14) . . . . ?
C31 P1 C41 C46 -20.05(16) . . . . ?
C31 C32 C33 C34 0.5(3) . . . . ?
C32 C31 C36 C35 -0.1(3) . . . . ?
C32 C33 C34 C35 -0.6(3) . . . . ?
C32 C33 C34 C37 177.20(18) . . . . ?
C33 C34 C35 C36 0.4(3) . . . . ?
C34 C35 C36 C31 -0.1(3) . . . . ?
C36 C31 C32 C33 -0.1(3) . . . . ?
C37 C34 C35 C36 -177.39(17) . . . . ?
C41 P1 O1 Mn1 -94.68(13) . . . . ?
C41 P1 C1 C2 175.38(12) . . . . ?
C41 P1 C1 C6 -1.63(15) . . . . ?
C41 P1 C31 C32 -85.52(15) . . . . ?
C41 P1 C31 C36 94.65(15) . . . . ?
C41 C42 C43 C44 -0.2(3) . . . . ?
C42 C41 C46 C45 -0.2(3) . . . . ?
C42 C43 C44 C45 -0.6(3) . . . . ?
C42 C43 C44 C47 177.91(19) . . . . ?
C43 C44 C45 C46 1.0(3) . . . . ?
C44 C45 C46 C41 -0.6(3) . . . . ?
C46 C41 C42 C43 0.7(3) . . . . ?
C47 C44 C45 C46 -177.48(18) . . . . ?

_olex2_submission_original_sample_id gard25q
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.847

####################################################################### 
# 
# 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_2-Re_gard25s
_database_code_depnum_ccdc_archive 'CCDC 2371549'
loop_
_audit_author_name
_audit_author_address
'James Gardinier'
;Marquette University
United States of America
;
_audit_update_record             
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_audit_creation_date             2024-03-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/1
loop_
_audit_author_email
james.gardinier@marquette.edu
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C30 H25 N4 O3 P Re, C F3 O3 S'
_chemical_formula_sum            'C31 H25 F3 N4 O6 P Re S'
_chemical_formula_weight         855.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         C31H25F3N4O6PReS
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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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                   8.9587(3)
_cell_length_b                   12.2629(4)
_cell_length_c                   14.9571(5)
_cell_angle_alpha                99.615(2)
_cell_angle_beta                 90.746(2)
_cell_angle_gamma                94.564(2)
_cell_volume                     1614.38(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14655
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6300
_cell_measurement_theta_min      4.3060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.027
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 1 1 0.0399
6 -1 -1 0.0479
0 7 2 0.0438
0 -7 -2 0.0010
-1 0 9 0.0152
1 0 -9 0.0182

_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.033
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
-6.0000 1.0000 1.0000 0.3933 0.9373 -0.2072
6.0000 -1.0000 -1.0000 -0.3933 -0.9373 0.2072
0.0000 7.0000 2.0000 -0.0849 -0.0942 -0.9443
-0.0000 -7.0000 -2.0000 0.0849 0.0942 0.9443
-1.0000 0.0000 9.0000 0.8469 -0.1579 -0.4043
1.0000 -0.0000 -9.0000 -0.8469 0.1579 0.4043

_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29459
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        70.622
_diffrn_reflns_theta_max         70.622
_diffrn_reflns_theta_min         3.668
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -10.00   1.00    9.62    --  -42.46 -77.00 -90.00  109
  2  ω    -92.00  -2.00   1.00    9.62    --  -42.46 125.00   0.00   90
  3  ω   -115.00 -14.00   1.00    9.62    --  -42.46 -57.00 150.00  101
  4  ω     27.00 126.00   1.00   38.49    --  100.00 -45.00   0.00   99
  5  ω     94.00 173.00   1.00   38.49    --  100.00 125.00  90.00   79
  6  ω     27.00 118.00   1.00   38.49    --  100.00-125.00  60.00   91
  7  ω     72.00 176.00   1.00   38.49    --  100.00  30.00 -60.00  104
  8  ω     27.00 118.00   1.00   38.49    --  100.00-125.00-150.00   91
  9  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 -90.00  109
 10  ω     74.00 173.00   1.00   38.49    --  100.00  45.00-120.00   99
 11  ω     74.00 173.00   1.00   38.49    --  100.00  45.00   0.00   99
 12  ω     94.00 173.00   1.00   38.49    --  100.00 125.00-120.00   79
 13  ω     27.00 118.00   1.00   38.49    --  100.00-125.00  90.00   91
 14  ω     27.00 118.00   1.00   38.49    --  100.00-125.00 -30.00   91
 15  ω     94.00 173.00   1.00   38.49    --  100.00 125.00-180.00   79
 16  ω     94.00 173.00   1.00   38.49    --  100.00 125.00 -60.00   79
 17  ω     24.00 133.00   1.00   38.49    --  100.00 -77.00-180.00  109
 18  ω   -115.00 -14.00   1.00    9.62    --  -42.46 -57.00 -30.00  101
 19  ω   -117.00 -18.00   1.00    9.62    --  -42.46 -37.00  30.00   99
 20  ω      1.00  83.00   1.00    9.62    --   42.46 -99.00 -90.00   82
 21  ω     10.00 119.00   1.00    9.62    --   42.46  77.00 150.00  109
 22  ω     71.00 172.00   1.00   38.49    --  100.00  61.00  30.00  101
 23  ω     71.00 172.00   1.00   38.49    --  100.00  61.00-180.00  101
 24  ω     47.00 178.00   1.00   38.49    --  100.00  15.00 150.00  131
 25  ω     67.00 176.00   1.00   38.49    --  100.00  77.00  60.00  109
 26  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 -60.00  109
 27  ω     67.00 155.00   1.00   38.49    --  100.00  77.00  90.00   88
 28  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 120.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0571269000
_diffrn_orient_matrix_UB_12      -0.0372032000
_diffrn_orient_matrix_UB_13      0.0877569000
_diffrn_orient_matrix_UB_21      -0.1627011000
_diffrn_orient_matrix_UB_22      -0.0032838000
_diffrn_orient_matrix_UB_23      -0.0356231000
_diffrn_orient_matrix_UB_31      0.0067868000
_diffrn_orient_matrix_UB_32      -0.1222818000
_diffrn_orient_matrix_UB_33      -0.0441662000
_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                5648
_reflns_number_total             6116
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.034
_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)+(0.0471P)²+2.4378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0881
_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 Ternary CH refined with riding coordinates:
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_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 0.35701(2) 0.63441(2) 0.24457(2) 0.02102(8) Uani 1 1 d . . . . .
P1 P 0.58689(11) 0.69558(8) 0.33887(7) 0.0195(2) Uani 1 1 d . . . . .
O3 O 0.0828(4) 0.5531(3) 0.1150(2) 0.0330(7) Uani 1 1 d . . . . .
O2 O 0.1334(4) 0.7416(3) 0.3791(2) 0.0353(7) Uani 1 1 d . . . . .
O1 O 0.2945(4) 0.4296(3) 0.3355(2) 0.0370(8) Uani 1 1 d . . . . .
N11 N 0.5017(4) 0.7895(3) 0.1159(2) 0.0230(7) Uani 1 1 d . . . . .
N12 N 0.3902(4) 0.7768(3) 0.1744(2) 0.0234(7) Uani 1 1 d . . . . .
N21 N 0.6298(4) 0.6227(3) 0.1116(2) 0.0222(7) Uani 1 1 d . . . . .
N22 N 0.5224(4) 0.5628(3) 0.1512(2) 0.0214(7) Uani 1 1 d . . . . .
C1 C 0.7230(5) 0.7939(3) 0.2972(3) 0.0226(8) Uani 1 1 d . . . . .
C2 C 0.7389(5) 0.8056(3) 0.2057(3) 0.0224(8) Uani 1 1 d . . . . .
C3 C 0.8465(5) 0.8851(3) 0.1836(3) 0.0252(9) Uani 1 1 d . . . . .
H3 H 0.857515 0.892319 0.123032 0.030 Uiso 1 1 calc R U . . .
C4 C 0.9378(5) 0.9538(4) 0.2495(3) 0.0284(9) Uani 1 1 d . . . . .
H4 H 1.007152 1.007296 0.233496 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9231(5) 0.9411(4) 0.3394(3) 0.0284(9) Uani 1 1 d . . . . .
H5 H 0.983320 0.985771 0.384457 0.034 Uiso 1 1 calc R U . . .
C6 C 0.8188(5) 0.8616(4) 0.3619(3) 0.0261(9) Uani 1 1 d . . . . .
H6 H 0.811876 0.852768 0.422299 0.031 Uiso 1 1 calc R U . . .
C7 C 0.6468(5) 0.7444(3) 0.1238(3) 0.0229(8) Uani 1 1 d . . . . .
H7 H 0.702186 0.761502 0.071076 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4734(5) 0.8681(4) 0.0657(3) 0.0286(9) Uani 1 1 d . . . . .
H11 H 0.534593 0.891860 0.021789 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3390(5) 0.9059(4) 0.0911(3) 0.0311(10) Uani 1 1 d . . . . .
H12 H 0.289882 0.959804 0.068327 0.037 Uiso 1 1 calc R U . . .
C13 C 0.2907(5) 0.8468(4) 0.1583(3) 0.0283(9) Uani 1 1 d . . . . .
H13 H 0.200888 0.854957 0.188190 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7172(5) 0.5549(4) 0.0599(3) 0.0280(9) Uani 1 1 d . . . . .
H21 H 0.797443 0.576727 0.026290 0.034 Uiso 1 1 calc R U . . .
C22 C 0.6670(5) 0.4484(4) 0.0655(3) 0.0304(10) Uani 1 1 d . . . . .
H22 H 0.705851 0.383687 0.037328 0.036 Uiso 1 1 calc R U . . .
C23 C 0.5443(5) 0.4571(4) 0.1227(3) 0.0273(9) Uani 1 1 d . . . . .
H23 H 0.486374 0.397200 0.138495 0.033 Uiso 1 1 calc R U . . .
C31 C 0.6969(5) 0.5799(3) 0.3508(3) 0.0213(8) Uani 1 1 d . . . . .
C32 C 0.8309(5) 0.5624(4) 0.3072(3) 0.0267(9) Uani 1 1 d . . . . .
H32 H 0.869312 0.612266 0.271161 0.032 Uiso 1 1 calc R U . . .
C33 C 0.9078(5) 0.4715(4) 0.3169(3) 0.0308(10) Uani 1 1 d . . . . .
H33 H 0.996624 0.460662 0.286411 0.037 Uiso 1 1 calc R U . . .
C34 C 0.8551(5) 0.3954(4) 0.3715(3) 0.0284(9) Uani 1 1 d . . . . .
C35 C 0.7200(5) 0.4122(4) 0.4139(3) 0.0264(9) Uani 1 1 d . . . . .
H35 H 0.682068 0.362283 0.450114 0.032 Uiso 1 1 calc R U . . .
C36 C 0.6404(5) 0.5020(4) 0.4033(3) 0.0243(8) Uani 1 1 d . . . . .
H36 H 0.548918 0.510609 0.431190 0.029 Uiso 1 1 calc R U . . .
C37 C 0.9428(6) 0.2981(4) 0.3840(4) 0.0405(12) Uani 1 1 d . . . . .
H37A H 0.995023 0.314006 0.441754 0.061 Uiso 1 1 calc R U . . .
H37B H 1.013686 0.285790 0.336556 0.061 Uiso 1 1 calc R U . . .
H37C H 0.875130 0.232849 0.381675 0.061 Uiso 1 1 calc R U . . .
C41 C 0.5554(5) 0.7638(3) 0.4543(3) 0.0214(8) Uani 1 1 d . . . . .
C42 C 0.6324(5) 0.7410(4) 0.5303(3) 0.0262(9) Uani 1 1 d . . . . .
H42 H 0.705712 0.690832 0.522891 0.031 Uiso 1 1 calc R U . . .
C43 C 0.5997(5) 0.7930(4) 0.6164(3) 0.0291(9) Uani 1 1 d . . . . .
H43 H 0.651742 0.777273 0.666315 0.035 Uiso 1 1 calc R U . . .
C44 C 0.4913(6) 0.8679(4) 0.6299(3) 0.0294(9) Uani 1 1 d . . . . .
C45 C 0.4176(5) 0.8937(4) 0.5537(3) 0.0270(9) Uani 1 1 d . . . . .
H45 H 0.346324 0.945433 0.561276 0.032 Uiso 1 1 calc R U . . .
C46 C 0.4504(5) 0.8425(3) 0.4670(3) 0.0245(8) Uani 1 1 d . . . . .
H46 H 0.401861 0.860902 0.416971 0.029 Uiso 1 1 calc R U . . .
C47 C 0.4491(7) 0.9187(5) 0.7242(3) 0.0406(12) Uani 1 1 d . . . . .
H47A H 0.431616 0.995159 0.725287 0.061 Uiso 1 1 calc R U . . .
H47B H 0.529193 0.914081 0.766322 0.061 Uiso 1 1 calc R U . . .
H47C H 0.359778 0.879283 0.740933 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1841(6) 0.5806(4) 0.1609(3) 0.0291(10) Uani 1 1 d . . . . .
C9 C 0.2180(5) 0.7038(4) 0.3298(3) 0.0270(9) Uani 1 1 d . . . . .
C8 C 0.3219(5) 0.5048(4) 0.3007(3) 0.0285(9) Uani 1 1 d . . . . .
S1 S 0.16872(12) 0.20968(9) 0.11721(7) 0.0256(2) Uani 1 1 d . . . . .
F1 F -0.0460(4) 0.2483(3) 0.0096(2) 0.0454(7) Uani 1 1 d . . . . .
F2 F -0.1039(5) 0.2663(4) 0.1488(3) 0.0753(13) Uani 1 1 d . . . . .
F3 F -0.0929(4) 0.1043(3) 0.0725(3) 0.0682(12) Uani 1 1 d . . . . .
O4 O 0.2193(5) 0.3247(3) 0.1254(3) 0.0557(12) Uani 1 1 d . . . . .
O5 O 0.2255(5) 0.1403(4) 0.0403(2) 0.0488(10) Uani 1 1 d . . . . .
O6 O 0.1688(4) 0.1642(3) 0.1994(2) 0.0347(7) Uani 1 1 d . . . . .
C14 C -0.0288(6) 0.2068(4) 0.0864(3) 0.0366(11) 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
Re1 P1 2.4734(10) . ?
Re1 N12 2.185(3) . ?
Re1 N22 2.183(4) . ?
Re1 C10 1.978(5) . ?
Re1 C9 1.936(5) . ?
Re1 C8 1.924(5) . ?
P1 C1 1.835(4) . ?
P1 C31 1.822(4) . ?
P1 C41 1.825(4) . ?
O3 C10 1.125(6) . ?
O2 C9 1.136(6) . ?
O1 C8 1.144(6) . ?
N11 N12 1.353(5) . ?
N11 C7 1.463(5) . ?
N11 C11 1.354(5) . ?
N12 C13 1.332(6) . ?
N21 N22 1.365(5) . ?
N21 C7 1.469(5) . ?
N21 C21 1.344(6) . ?
N22 C23 1.326(6) . ?
C1 C2 1.407(6) . ?
C1 C6 1.399(6) . ?
C2 C3 1.399(6) . ?
C2 C7 1.521(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.360(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(7) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.364(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.402(7) . ?
C23 H23 0.9300 . ?
C31 C32 1.389(6) . ?
C31 C36 1.403(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.383(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.398(6) . ?
C34 C35 1.388(7) . ?
C34 C37 1.515(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(6) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.401(6) . ?
C41 C46 1.393(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.385(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(7) . ?
C44 C45 1.403(6) . ?
C44 C47 1.509(7) . ?
C45 H45 0.9300 . ?
C45 C46 1.389(6) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
S1 O4 1.432(4) . ?
S1 O5 1.436(4) . ?
S1 O6 1.432(3) . ?
S1 C14 1.818(5) . ?
F1 C14 1.344(6) . ?
F2 C14 1.313(7) . ?
F3 C14 1.321(6) . ?

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
N12 Re1 P1 91.27(10) . . ?
N22 Re1 P1 80.72(9) . . ?
N22 Re1 N12 84.38(13) . . ?
C10 Re1 P1 175.23(13) . . ?
C10 Re1 N12 87.80(15) . . ?
C10 Re1 N22 94.53(16) . . ?
C9 Re1 P1 96.76(13) . . ?
C9 Re1 N12 94.29(16) . . ?
C9 Re1 N22 177.11(16) . . ?
C9 Re1 C10 87.97(18) . . ?
C8 Re1 P1 91.48(13) . . ?
C8 Re1 N12 176.94(16) . . ?
C8 Re1 N22 94.74(16) . . ?
C8 Re1 C10 89.35(18) . . ?
C8 Re1 C9 86.73(19) . . ?
C1 P1 Re1 116.94(13) . . ?
C31 P1 Re1 111.88(13) . . ?
C31 P1 C1 103.08(19) . . ?
C31 P1 C41 105.53(18) . . ?
C41 P1 Re1 115.00(14) . . ?
C41 P1 C1 103.04(19) . . ?
N12 N11 C7 122.6(3) . . ?
N12 N11 C11 110.7(4) . . ?
C11 N11 C7 125.0(4) . . ?
N11 N12 Re1 123.8(3) . . ?
C13 N12 Re1 128.2(3) . . ?
C13 N12 N11 105.4(3) . . ?
N22 N21 C7 124.5(3) . . ?
C21 N21 N22 110.7(3) . . ?
C21 N21 C7 124.8(4) . . ?
N21 N22 Re1 124.8(3) . . ?
C23 N22 Re1 129.4(3) . . ?
C23 N22 N21 105.7(4) . . ?
C2 C1 P1 125.1(3) . . ?
C6 C1 P1 117.0(3) . . ?
C6 C1 C2 117.9(4) . . ?
C1 C2 C7 127.9(4) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 C7 112.9(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 118.7 . . ?
C5 C6 C1 122.5(4) . . ?
C5 C6 H6 118.7 . . ?
N11 C7 N21 111.0(3) . . ?
N11 C7 C2 112.1(3) . . ?
N11 C7 H7 105.0 . . ?
N21 C7 C2 117.4(3) . . ?
N21 C7 H7 105.0 . . ?
C2 C7 H7 105.0 . . ?
N11 C11 H11 126.2 . . ?
N11 C11 C12 107.5(4) . . ?
C12 C11 H11 126.2 . . ?
C11 C12 H12 127.3 . . ?
C11 C12 C13 105.3(4) . . ?
C13 C12 H12 127.3 . . ?
N12 C13 C12 111.0(4) . . ?
N12 C13 H13 124.5 . . ?
C12 C13 H13 124.5 . . ?
N21 C21 H21 126.2 . . ?
N21 C21 C22 107.7(4) . . ?
C22 C21 H21 126.2 . . ?
C21 C22 H22 127.3 . . ?
C21 C22 C23 105.4(4) . . ?
C23 C22 H22 127.3 . . ?
N22 C23 C22 110.4(4) . . ?
N22 C23 H23 124.8 . . ?
C22 C23 H23 124.8 . . ?
C32 C31 P1 123.1(3) . . ?
C32 C31 C36 118.3(4) . . ?
C36 C31 P1 118.5(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(4) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.2 . . ?
C32 C33 C34 121.5(4) . . ?
C34 C33 H33 119.2 . . ?
C33 C34 C37 121.1(4) . . ?
C35 C34 C33 117.8(4) . . ?
C35 C34 C37 121.2(4) . . ?
C34 C35 H35 119.4 . . ?
C34 C35 C36 121.2(4) . . ?
C36 C35 H35 119.4 . . ?
C31 C36 H36 119.7 . . ?
C35 C36 C31 120.5(4) . . ?
C35 C36 H36 119.7 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 P1 123.0(3) . . ?
C46 C41 P1 118.2(3) . . ?
C46 C41 C42 118.8(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 C41 120.1(4) . . ?
C43 C42 H42 119.9 . . ?
C42 C43 H43 119.3 . . ?
C44 C43 C42 121.5(4) . . ?
C44 C43 H43 119.3 . . ?
C43 C44 C45 118.5(4) . . ?
C43 C44 C47 121.2(4) . . ?
C45 C44 C47 120.3(4) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.4(4) . . ?
C46 C45 H45 119.8 . . ?
C41 C46 H46 119.7 . . ?
C45 C46 C41 120.7(4) . . ?
C45 C46 H46 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C10 Re1 177.4(4) . . ?
O2 C9 Re1 177.8(4) . . ?
O1 C8 Re1 176.6(4) . . ?
O4 S1 O5 114.2(3) . . ?
O4 S1 O6 116.1(2) . . ?
O4 S1 C14 103.2(3) . . ?
O5 S1 C14 102.2(3) . . ?
O6 S1 O5 114.6(2) . . ?
O6 S1 C14 104.1(2) . . ?
F1 C14 S1 110.6(4) . . ?
F2 C14 S1 112.5(4) . . ?
F2 C14 F1 106.7(4) . . ?
F2 C14 F3 107.9(5) . . ?
F3 C14 S1 111.3(4) . . ?
F3 C14 F1 107.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 P1 C1 C2 -25.3(4) . . . . ?
Re1 P1 C1 C6 155.2(3) . . . . ?
Re1 P1 C31 C32 107.1(4) . . . . ?
Re1 P1 C31 C36 -70.0(3) . . . . ?
Re1 P1 C41 C42 136.2(3) . . . . ?
Re1 P1 C41 C46 -44.1(4) . . . . ?
Re1 N12 C13 C12 -163.0(3) . . . . ?
Re1 N22 C23 C22 -177.7(3) . . . . ?
P1 C1 C2 C3 179.2(3) . . . . ?
P1 C1 C2 C7 2.3(6) . . . . ?
P1 C1 C6 C5 -178.1(4) . . . . ?
P1 C31 C32 C33 -178.3(4) . . . . ?
P1 C31 C36 C35 179.7(3) . . . . ?
P1 C41 C42 C43 -177.9(3) . . . . ?
P1 C41 C46 C45 177.4(3) . . . . ?
N11 N12 C13 C12 -1.1(5) . . . . ?
N11 C11 C12 C13 0.3(5) . . . . ?
N12 N11 C7 N21 63.4(5) . . . . ?
N12 N11 C7 C2 -70.1(5) . . . . ?
N12 N11 C11 C12 -1.1(5) . . . . ?
N21 N22 C23 C22 0.7(5) . . . . ?
N21 C21 C22 C23 0.5(5) . . . . ?
N22 N21 C7 N11 -45.0(5) . . . . ?
N22 N21 C7 C2 85.7(5) . . . . ?
N22 N21 C21 C22 -0.1(5) . . . . ?
C1 P1 C31 C32 -19.4(4) . . . . ?
C1 P1 C31 C36 163.5(3) . . . . ?
C1 P1 C41 C42 -95.4(4) . . . . ?
C1 P1 C41 C46 84.3(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C7 N11 78.2(5) . . . . ?
C1 C2 C7 N21 -52.0(6) . . . . ?
C2 C1 C6 C5 2.4(6) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C2 C7 N11 -98.9(4) . . . . ?
C3 C2 C7 N21 130.9(4) . . . . ?
C3 C4 C5 C6 -0.4(7) . . . . ?
C4 C5 C6 C1 -1.5(7) . . . . ?
C6 C1 C2 C3 -1.3(6) . . . . ?
C6 C1 C2 C7 -178.3(4) . . . . ?
C7 N11 N12 Re1 -29.9(5) . . . . ?
C7 N11 N12 C13 167.2(4) . . . . ?
C7 N11 C11 C12 -166.5(4) . . . . ?
C7 N21 N22 Re1 -2.1(5) . . . . ?
C7 N21 N22 C23 179.4(4) . . . . ?
C7 N21 C21 C22 -179.9(4) . . . . ?
C7 C2 C3 C4 176.9(4) . . . . ?
C11 N11 N12 Re1 164.2(3) . . . . ?
C11 N11 N12 C13 1.4(5) . . . . ?
C11 N11 C7 N21 -132.8(4) . . . . ?
C11 N11 C7 C2 93.7(5) . . . . ?
C11 C12 C13 N12 0.5(5) . . . . ?
C21 N21 N22 Re1 178.2(3) . . . . ?
C21 N21 N22 C23 -0.3(4) . . . . ?
C21 N21 C7 N11 134.7(4) . . . . ?
C21 N21 C7 C2 -94.5(5) . . . . ?
C21 C22 C23 N22 -0.8(5) . . . . ?
C31 P1 C1 C2 97.9(4) . . . . ?
C31 P1 C1 C6 -81.6(4) . . . . ?
C31 P1 C41 C42 12.4(4) . . . . ?
C31 P1 C41 C46 -168.0(3) . . . . ?
C31 C32 C33 C34 -0.9(7) . . . . ?
C32 C31 C36 C35 2.4(6) . . . . ?
C32 C33 C34 C35 1.9(7) . . . . ?
C32 C33 C34 C37 -178.0(5) . . . . ?
C33 C34 C35 C36 -0.6(7) . . . . ?
C34 C35 C36 C31 -1.5(7) . . . . ?
C36 C31 C32 C33 -1.2(7) . . . . ?
C37 C34 C35 C36 179.3(5) . . . . ?
C41 P1 C1 C2 -152.5(4) . . . . ?
C41 P1 C1 C6 28.1(4) . . . . ?
C41 P1 C31 C32 -127.2(4) . . . . ?
C41 P1 C31 C36 55.8(4) . . . . ?
C41 C42 C43 C44 0.1(7) . . . . ?
C42 C41 C46 C45 -3.0(6) . . . . ?
C42 C43 C44 C45 -2.2(7) . . . . ?
C42 C43 C44 C47 176.0(5) . . . . ?
C43 C44 C45 C46 1.8(7) . . . . ?
C44 C45 C46 C41 0.8(7) . . . . ?
C46 C41 C42 C43 2.5(7) . . . . ?
C47 C44 C45 C46 -176.5(5) . . . . ?
O4 S1 C14 F1 58.0(4) . . . . ?
O4 S1 C14 F2 -61.2(5) . . . . ?
O4 S1 C14 F3 177.5(4) . . . . ?
O5 S1 C14 F1 -60.8(4) . . . . ?
O5 S1 C14 F2 180.0(4) . . . . ?
O5 S1 C14 F3 58.7(4) . . . . ?
O6 S1 C14 F1 179.6(4) . . . . ?
O6 S1 C14 F2 60.4(4) . . . . ?
O6 S1 C14 F3 -60.8(4) . . . . ?

_olex2_submission_original_sample_id gard25s
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.841
