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_4127492
_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         'C31 H34 Cl Cr P'
_chemical_formula_sum            'C31 H34 Cl Cr P'
_chemical_formula_weight         525.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.230(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1380(2)
_cell_length_b                   18.3287(4)
_cell_length_c                   16.6855(4)
_cell_measurement_reflns_used    19398
_cell_measurement_temperature    180.0(2)
_cell_measurement_theta_max      30.3880
_cell_measurement_theta_min      3.8110
_cell_volume                     2758.43(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.0(2)
_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      2.00  31.00   0.50    3.34    --   -1.60 -82.00 120.00   58
  2  \w    -33.00  31.00   0.50    3.34    --   -1.60 -82.00   0.00  128
  3  \w    -24.00   2.00   0.50    3.34    --   -1.60  57.00 -30.00   52
  4  \w    -23.00  74.00   0.50    3.34    --   -1.60  57.00 150.00  194
  5  \w     37.00  85.00   0.50    3.34    --   -1.60  38.00  30.00   96
  6  \w      4.00  29.00   0.50    3.34    --   -1.60 -77.00 -90.00   50
  7  \w     22.00  83.00   0.50    3.34    --    1.90  19.00  90.00  122
  8  \w    -21.00  30.00   0.50    3.34    --    1.90  57.00-150.00  102
  9  \w    -62.00 -36.00   0.50    3.34    --    1.90 -38.00 150.00   52
 10  \w     61.00  87.00   0.50    3.34    --    1.90  57.00-150.00   52
 11  \w    -12.00  -6.50   0.50    3.34    --    1.90  38.00   0.00   11
;
_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      0.0324993000
_diffrn_orient_matrix_UB_12      -0.0328210000
_diffrn_orient_matrix_UB_13      0.0168827000
_diffrn_orient_matrix_UB_21      0.0014170000
_diffrn_orient_matrix_UB_22      -0.0137198000
_diffrn_orient_matrix_UB_23      -0.0396150000
_diffrn_orient_matrix_UB_31      0.0716297000
_diffrn_orient_matrix_UB_32      0.0151975000
_diffrn_orient_matrix_UB_33      0.0007167000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.531
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80520
_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            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0390P)^2^+1.2210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5002
_reflns_number_total             5416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00822_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4127492
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 P1 Cr1 Cl1 O1'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.933
_reflns_odcompleteness_completeness 99.66
_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 Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_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 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.718