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_4134835
_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         'C36 H65 Cr3 N2 Si3'
_chemical_formula_sum            'C36 H65 Cr3 N2 Si3'
_chemical_formula_weight         766.17
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.239(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.955(10)
_cell_length_b                   10.840(3)
_cell_length_c                   19.797(6)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.28
_cell_volume                     8139(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            102352
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.611
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.6968
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1664 before and 0.1225 after correction. The Ratio of minimum to maximum transmission is 0.7989. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       plate
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         14303
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+47.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10671
_reflns_number_total             14303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02939_si_003.cif
_cod_data_source_block           Complex7_26018ts
_cod_database_code               4134835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si3-C34 \\sim Si3-C34A
 with sigma of 0.02
 Si3-C36 \\sim Si3-C36A
 with sigma of 0.02
 Si3-C35 \\sim Si3-C35A
 with sigma of 0.02
3. Others
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36A)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=Sof(C35A)=Sof(H35A)=Sof(H3)=Sof(H4)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=
 Sof(C36)=Sof(H3AD)=Sof(H3AE)=Sof(H3AF)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H), N4(HA)
4.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), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C42(HB,HC,HD), C43(HE,HF,HG), C44(HH,HI,HJ), C45(HK,HL,HM), C46(HN,HO,HP),
 C47(HQ,HR,HS), C48(HT,HU,HV), C54(HW,HX,HY), C55(HZ,H1AA,H2AA), C56(H4AA,H5AA,
 H6AA), C57(H7AA,H8AA,H9AA), C58(H0BA,H1BA,H2BA), C59(H3BA,H4BA,H5BA), C60(H6BA,
 H7BA,H8BA), C66(H9BA,H0CA,H1CA), C67(H2CA,H3CA,H4CA), C68(H5CA,H6CA,H7CA),
 C69(H8CA,H9CA,H0DA), C70(H1DA,H2DA,H3DA), C71(H4DA,H5DA,H6DA), C72(H7DA,H8DA,
 H9DA), C35(H0AA,H0AB,H0AC), C36(H3AD,H3AE,H3AF), C34A(H34D,H34E,H34F),
 C36A(H36A,H36B,H36C), C35A(H35A,H3,H4)
;
_shelx_res_checksum              29565
_shelx_hkl_checksum              77287
_olex2_submission_special_instructions 'No special instructions were received'