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_1565105
_publ_section_title
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 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         'C54 H76 Cr3 N8 Si3, C4 H10 O1'
_chemical_formula_sum            'C58 H86 Cr3 N8 O Si3'
_chemical_formula_weight         1151.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                104.1910(10)
_cell_angle_beta                 90.5520(10)
_cell_angle_gamma                105.9240(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4743(5)
_cell_length_b                   14.4695(7)
_cell_length_c                   17.6459(8)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.55
_cell_measurement_theta_min      2.23
_cell_volume                     2959.2(2)
_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 0.981
_diffrn_measured_fraction_theta_max 0.978
_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  0.1055
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62323
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.568
_diffrn_reflns_theta_min         0.971
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1668 before and 0.0873 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       'medium rectangular block'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         13259
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0377P)^2^+2.1281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9556
_reflns_number_total             13259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04819h2.cif
_cod_data_source_block           tbsLCr3NPh_2
_cod_database_code               1565105
_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. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C29A)
Uanis(C28) = Uanis(C28A)
Uanis(C30) = Uanis(C30A)
Uanis(O8) = Uanis(O7)
Uanis(C82) = Uanis(C72)
Uanis(C81) = Uanis(C71)
Uanis(C83) = Uanis(C73)
Uanis(C84) = Uanis(C74)
3. Same fragment restrains
{C81, C82, O8, C83, C84} sigma for 1-2: 0.02, 1-3: 0.04
as
{C71, C72, O7, C73, C74}
4. Others
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(3)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(O7)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=1-FVAR(4)
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(O8)=
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C4AA(H4AA), C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5AA(H5AA,H5AB), C6(H6A,H6B), C72(H72A,H72B), C73(H73A,H73B),
 C82(H82A,H82B), C83(H83A,H83B)
5.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), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C28A(H28D,H28E,
 H28F), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F), C30(H30A,H30B,H30C),
 C30A(H30D,H30E,H30F), 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), C40A(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42A(H42A,H42B,H42C),
 C71(H71A,H71B,H71C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C), C84(H84A,H84B,
 H84C)
;
_olex2_submission_special_instructions 'No special instructions were received'