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_4127493
_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 H46 Cl Cr P'
_chemical_formula_sum            'C31 H46 Cl Cr P'
_chemical_formula_weight         537.10
_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                 99.642(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8191(3)
_cell_length_b                   16.7850(3)
_cell_length_c                   16.1306(4)
_cell_measurement_reflns_used    14574
_cell_measurement_temperature    179.99(14)
_cell_measurement_theta_max      29.2630
_cell_measurement_theta_min      3.6470
_cell_volume                     2887.91(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -32.00  43.00   0.50    2.00    --  -15.70 -38.00-120.00  150
  2  \w    -15.00  30.00   0.50    2.00    --  -15.70 -82.00 -30.00   90
  3  \w    -41.00 -13.00   0.50    2.00    --  -15.70  77.00  60.00   56
  4  \w    -49.00  67.00   0.50    2.00    --  -15.70  57.00 -90.00  232
  5  \w    -56.00 -30.00   0.50    2.00    --  -15.70  77.00-120.00   52
  6  \w    -18.00  33.00   0.50    2.00    --   15.80 -82.00 150.00  102
  7  \w    -13.00 102.00   0.50    2.00    --   15.80  57.00  30.00  230
  8  \w    -74.00  27.00   0.50    2.00    --   15.80 -57.00  90.00  202
  9  \w    -25.00  61.00   0.50    2.00    --   15.80 -82.00-180.00  172
;
_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      -0.0321527000
_diffrn_orient_matrix_UB_12      -0.0357006000
_diffrn_orient_matrix_UB_13      -0.0135959000
_diffrn_orient_matrix_UB_21      0.0580804000
_diffrn_orient_matrix_UB_22      -0.0203376000
_diffrn_orient_matrix_UB_23      0.0034935000
_diffrn_orient_matrix_UB_31      -0.0033472000
_diffrn_orient_matrix_UB_32      -0.0098494000
_diffrn_orient_matrix_UB_33      0.0423673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31931
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74410
_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 dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.784
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0876P)^2^+4.6683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4696
_reflns_number_total             5675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00822_si_002.cif
_cod_data_source_block           2b
_cod_database_code               4127493
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Cr C H P Cl'
_chemical_oxdiff_usercomment     zyh180501f,Zn,epN3
_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. Others
 Sof(P1)=Sof(C0AA)=Sof(H0AA)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C5AA)=Sof(H5AA)=
 Sof(H5AB)=Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=Sof(H20A)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=1-FVAR(1)
 Sof(P2)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=Sof(H20)=
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C0AA(H0AA), C20(H20), C20(H20A), C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C4AA(H4AA,H4AB), C5AA(H5AA,H5AB), C6(H6A,H6B), C7AA(H7AA,
 H7AB), C8(H8A,H8B), C8AA(H8AA,H8AB), C10(H10A,H10B), C12(H12A,H12B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18)
3.d 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 4.472
_oxdiff_exptl_absorpt_empirical_full_min 0.614