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_4127494
_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         'C25 H38 Cl Cr P'
_chemical_formula_sum            'C25 H38 Cl Cr P'
_chemical_formula_weight         456.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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
_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                74.282(2)
_cell_angle_beta                 84.815(2)
_cell_angle_gamma                86.464(2)
_cell_formula_units_Z            4
_cell_length_a                   8.4943(2)
_cell_length_b                   17.3964(5)
_cell_length_c                   17.6923(5)
_cell_measurement_reflns_used    15967
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.3160
_cell_measurement_theta_min      3.7710
_cell_volume                     2504.45(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -47.00  14.00   0.50    1.20    --   -5.20 -77.00 -30.00  122
  2  \w    -32.00   6.00   0.50    1.20    --   -5.20 -82.00 150.00   76
  3  \w    -27.00  -1.00   0.50    1.20    --   -5.20 -82.00-180.00   52
  4  \w     14.00  42.00   0.50    1.20    --    5.20 -82.00  60.00   56
  5  \w      6.00  35.00   0.50    1.20    --    5.20 -82.00-120.00   58
  6  \w    -32.00  -2.00   0.50    1.20    --    5.20 -82.00  30.00   60
  7  \w    -21.00  57.00   0.50    1.20    --    5.20  43.00 -32.58  156
  8  \w    -32.00  95.00   0.50    1.20    --    5.20  19.00  60.00  254
  9  \w    -27.00   0.00   0.50    1.20    --    5.20 -82.00  90.00   54
 10  \w    -22.00  74.00   0.50    1.20    --    5.20  38.00-180.00  192
;
_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      0.0234509000
_diffrn_orient_matrix_UB_12      -0.0258266000
_diffrn_orient_matrix_UB_13      -0.0242255000
_diffrn_orient_matrix_UB_21      -0.0177061000
_diffrn_orient_matrix_UB_22      -0.0335735000
_diffrn_orient_matrix_UB_23      0.0321814000
_diffrn_orient_matrix_UB_31      -0.0785958000
_diffrn_orient_matrix_UB_32      0.0016132000
_diffrn_orient_matrix_UB_33      -0.0110593000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45628
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.478
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         11418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.5502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9411
_reflns_number_total             11418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00822_si_002.cif
_cod_data_source_block           2c
_cod_database_code               4127494
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H P Cl Cr'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.951
_reflns_odcompleteness_completeness 99.58
_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:
 C20(H20), C23(H23), C45(H45), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C31(H31A,H31B),
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C40(H40), C41(H41), C42(H42), C43(H43)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C)
;
_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 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.428