Revealing Redox Isomerism in Trichromium Imides by Anomalous Diffraction
Bartholomew, Amymarie K.; Chen, Yu-Sheng; Grass Wang, Suyin; Bu, Wei; Dong, Yuyang; Juda, Cristin E.; Betley, Theodore; Anderton, Kevin J.; Musgrave, Rebecca A.; Chemical Science  (2021) –; doi:10.1039/D1SC04819H

data_1565104
_publ_section_title
;
 Revealing Redox Isomerism in Trichromium Imides by Anomalous Diffraction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04819H
_journal_year                    2021
_chemical_formula_moiety         'C50 H73 Cr3 N7 Si3, C6 H6'
_chemical_formula_sum            'C56 H79 Cr3 N7 Si3'
_chemical_formula_weight         1090.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2019-08-26 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3541(5)
_cell_length_b                   29.4601(11)
_cell_length_c                   14.0800(5)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.56
_cell_measurement_theta_min      2.33
_cell_volume                     5530.2(4)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS,2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            115483
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         16.403
_diffrn_reflns_theta_min         0.888
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1051 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.8719.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       'medium rectangular block'
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.186
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         12565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0398
_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/[\s^2^(Fo^2^)+(0.0535P)^2^+3.9017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9983
_reflns_number_total             12565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04819h2.cif
_cod_data_source_block           tbsLCr3CNBn
_cod_database_code               1565104
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'