Dinitrogen Activation and Hydrogenation by C<sub>5</sub>Me<sub>4</sub>SiMe<sub>3</sub>-Ligated Di- and Trinuclear Chromium Hydride Complexes.
Shima, Takanori; Yang, Jimin; Luo, Gen; Luo, Yi; Hou, Zhaomin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02939

data_4134833
_publ_section_title
;
 Dinitrogen Activation and Hydrogenation by
 C<sub>5</sub>Me<sub>4</sub>SiMe<sub>3</sub>-Ligated Di- and Trinuclear
 Chromium Hydride Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02939
_journal_year                    2020
_chemical_formula_moiety         'C48 H86 Cr4 N2 Si4'
_chemical_formula_sum            'C48 H86 Cr4 N2 Si4'
_chemical_formula_weight         1011.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.350(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.9967(11)
_cell_length_b                   11.1756(4)
_cell_length_c                   32.7459(13)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.50
_cell_volume                     10580.9(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9936
_diffrn_measured_fraction_theta_max 0.9936
_diffrn_measurement_device_type  'CMOS area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            106333
_diffrn_reflns_theta_full        27.9418
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.2699
_exptl_crystal_description       plate
_exptl_crystal_F_000             4333.8582
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5277
_refine_diff_density_min         -0.4953
_refine_diff_density_rms         0.1232
_refine_ls_d_res_high            0.7584
_refine_ls_d_res_low             10.4374
_refine_ls_goodness_of_fit_ref   1.0511
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    111
_refine_ls_number_parameters     562
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0511
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+11.8604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              38
_reflns_limit_h_min              -38
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              43
_reflns_limit_l_min              0
_reflns_number_gt                9636
_reflns_number_total             12640
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c02939_si_003.cif
_cod_data_source_block           Complex5isomer_26136ts
_cod_database_code               4134833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b)
2.b Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C18(H18a,H18b,H18c),
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C30(H30a,H30b,H30c), C31(H31a,
 H31b,H31c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c),
 C36(H36a,H36b,H36c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,
 H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,
 H48b,H48c)
;
_olex2_submission_special_instructions 'No special instructions were received'