Dinitrogen Functionalization Affording Chromium Hydrazido Complex.
Yin, Jianhao; Li, Jiapeng; Wang, Gao-Xiang; Yin, Zhu-Bao; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 141 (2019) 4241–4247; doi:10.1021/jacs.9b00822

data_4127500
_publ_section_title
;
 Dinitrogen Functionalization Affording Chromium Hydrazido Complex.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4241
_journal_page_last               4247
_journal_paper_doi               10.1021/jacs.9b00822
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C37 H64 Cr N2 P Si2'
_chemical_formula_sum            'C37 H64 Cr N2 P Si2'
_chemical_formula_weight         676.05
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.867(2)
_cell_angle_beta                 101.725(3)
_cell_angle_gamma                103.420(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8222(4)
_cell_length_b                   11.3035(4)
_cell_length_c                   16.5127(3)
_cell_measurement_reflns_used    16893
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.1510
_cell_measurement_theta_min      3.7910
_cell_volume                     1919.70(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -25.00  88.00   0.50    5.92    --   -1.40  20.00  76.53  226
  2  \w    -26.00  85.00   0.50    5.92    --   -1.40  19.00 -30.00  222
  3  \w     57.00  83.00   0.50    5.92    --   -1.40  19.00-150.00   52
  4  \w    -26.00  40.00   0.50    5.92    --   -1.40  19.00-150.00  132
  5  \w    -32.00  34.00   0.50    5.92    --    1.60 -82.00 -60.00  132
  6  \w    -35.00  26.00   0.50    5.92    --    1.60 -59.00 178.84  122
  7  \w    -33.00  32.00   0.50    5.92    --    1.60 -77.00-120.00  130
  8  \w      9.00  34.00   0.50    5.92    --    1.60 -82.00  60.00   50
  9  \w    -45.00  32.00   0.50    5.92    --    1.60 -77.00 120.00  154
 10  \w    -33.00  34.00   0.50    5.92    --    1.60 -82.00   0.00  134
 11  \w    -85.00 -60.00   0.50    5.92    --    1.60 -59.00 178.84   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0057445000
_diffrn_orient_matrix_UB_12      -0.0363437000
_diffrn_orient_matrix_UB_13      0.0343109000
_diffrn_orient_matrix_UB_21      -0.0557956000
_diffrn_orient_matrix_UB_22      -0.0405363000
_diffrn_orient_matrix_UB_23      -0.0243148000
_diffrn_orient_matrix_UB_31      0.0401238000
_diffrn_orient_matrix_UB_32      -0.0348728000
_diffrn_orient_matrix_UB_33      -0.0128275000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45403
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.525
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.911
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 5929 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.146(12)
_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     795
_refine_ls_number_reflns         14717
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1278P)^2^+1.5264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1846
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                13720
_reflns_number_total             14717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00822_si_002.cif
_cod_data_source_block           5
_cod_database_code               4127500
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H P Cr N Si'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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:
 C12(H12), C18(H18), C49(H49), C55(H55)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B),
  C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,H65B), C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C39(H39), C40(H40), C41(H41), C42(H42)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C62(H62A,H62B,H62C),
 C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C)
;
_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 1.766
_oxdiff_exptl_absorpt_empirical_full_min 0.616