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_4127499
_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         'C49 H82 Cr Cs N6 O6 P'
_chemical_formula_sum            'C49 H82 Cr Cs N6 O6 P'
_chemical_formula_weight         1067.08
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 93.673(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3634(4)
_cell_length_b                   18.6014(3)
_cell_length_c                   24.1640(4)
_cell_measurement_reflns_used    72769
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.5830
_cell_measurement_theta_min      3.6830
_cell_volume                     11377.0(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(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    -22.00  16.00   0.50   21.00    --   -1.70 -82.00  30.00   76
  2  \w    -20.00  30.00   0.50   21.00    --   -1.70 -82.00 -90.00  100
  3  \w     -8.00  88.00   0.50   21.00    --   -1.70  57.00  60.00  192
  4  \w    -33.00  29.00   0.50   21.00    --   -1.70 -82.00-120.00  124
  5  \w    -91.00  15.00   0.50   21.00    --   -1.70 -37.00  60.00  212
  6  \w    -61.00 -35.00   0.50   21.00    --    1.90   0.00  30.00   52
  7  \w     38.00  90.00   0.50   21.00    --    1.90  37.00  30.00  104
  8  \w     29.00  54.00   0.50   21.00    --    1.90  37.00  90.00   50
  9  \w    -18.00  36.00   0.50   21.00    --    1.90  57.00  30.00  108
 10  \w    -45.00   8.00   0.50   21.00    --    1.90 -57.00   0.00  106
 11  \w      9.00  70.00   0.50   21.00    --    1.90   0.00  30.00  122
;
_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      0.0021477000
_diffrn_orient_matrix_UB_12      -0.0173722000
_diffrn_orient_matrix_UB_13      -0.0258831000
_diffrn_orient_matrix_UB_21      -0.0264147000
_diffrn_orient_matrix_UB_22      0.0098007000
_diffrn_orient_matrix_UB_23      -0.0080549000
_diffrn_orient_matrix_UB_31      0.0091277000
_diffrn_orient_matrix_UB_32      0.0324909000
_diffrn_orient_matrix_UB_33      -0.0114191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            263705
_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         27.485
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54136
_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 green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         26015
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+12.0663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23917
_reflns_number_total             26015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00822_si_002.cif
_cod_data_source_block           4c
_cod_database_code               4127499
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H P O Cr Cs N'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.915
_reflns_odcompleteness_completeness 99.68
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H79A-H0AB
 2.1 with sigma of 0.01
 H98A-H72D
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C19 \\sim C32 \\sim C50 \\sim C26 \\sim C1 \\sim C45 \\sim C3 \\sim C14 \\sim
C2 \\sim C36 \\sim C5 \\sim C4 \\sim C57 \\sim C25 \\sim C52 \\sim C46 \\sim
C33 \\sim C51 \\sim C18 \\sim C62 \\sim C15 \\sim C54 \\sim C31 \\sim C6 \\sim
C56 \\sim C20 \\sim C47 \\sim C34 \\sim C53 \\sim C8 \\sim C37 \\sim C35 \\sim
C10 \\sim C43 \\sim C60 \\sim C55 \\sim C24 \\sim C30 \\sim C82 \\sim C81 \\sim
C12 \\sim C49 \\sim C11 \\sim C59 \\sim C29 \\sim C27 \\sim C58 \\sim C48 \\sim
C17 \\sim C28 \\sim C98 \\sim C61 \\sim C41 \\sim C16 \\sim C97 \\sim C21 \\sim
C84 \\sim C9 \\sim C13 \\sim C39 \\sim C83 \\sim C87 \\sim C74 \\sim C38 \\sim
C42 \\sim C63 \\sim C22 \\sim C23 \\sim C96 \\sim C68 \\sim C7 \\sim C88 \\sim
C85 \\sim C80 \\sim C75 \\sim C95 \\sim C44 \\sim C90 \\sim C93 \\sim C73 \\sim
C40 \\sim C64 \\sim C89 \\sim C66 \\sim C94 \\sim C76 \\sim C67 \\sim C69 \\sim
C65 \\sim C86 \\sim C70 \\sim C91 \\sim C92 \\sim C79 \\sim C72A \\sim C77
\\sim C78A \\sim C71A \\sim C78B \\sim C72B \\sim C71B \\sim C0AA: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H69C)=Sof(H69D)=Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78C)=Sof(H78D)=
 Sof(C72B)=Sof(H72C)=Sof(H72D)=Sof(C71B)=Sof(H71C)=Sof(H71D)=Sof(C0AA)=
 Sof(H0AA)=Sof(H0AB)=1-FVAR(1)
 Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C72A)=Sof(H72A)=
 Sof(H72B)=Sof(H77A)=Sof(H77B)=Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(C71A)=
 Sof(H71A)=Sof(H71B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C57(H57), C25(H25), C51(H51)
5.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C62(H62A,H62B), C54(H54A,H54B), C31(H31A,H31B), C6(H6A,H6B),
 C56(H56A,H56B), C20(H20A,H20B), C53(H53A,H53B), C8(H8A,H8B), C37(H37A,H37B),
 C10(H10A,H10B), C43(H43A,H43B), C60(H60A,H60B), C55(H55A,H55B), C24(H24A,H24B),
  C30(H30A,H30B), C82(H82A,H82B), C81(H81A,H81B), C12(H12A,H12B), C59(H59A,
 H59B), C29(H29A,H29B), C27(H27A,H27B), C58(H58A,H58B), C28(H28A,H28B),
 C98(H98A,H98B), C61(H61A,H61B), C41(H41A,H41B), C97(H97A,H97B), C21(H21A,H21B),
  C39(H39A,H39B), C83(H83A,H83B), C87(H87A,H87B), C74(H74A,H74B), C22(H22A,
 H22B), C23(H23A,H23B), C96(H96A,H96B), C88(H88A,H88B), C85(H85A,H85B),
 C80(H80A,H80B), C75(H75A,H75B), C90(H90A,H90B), C93(H93A,H93B), C73(H73A,H73B),
  C64(H64A,H64B), C89(H89A,H89B), C66(H66A,H66B), C94(H94A,H94B), C76(H76A,
 H76B), C67(H67A,H67B), C69(H69A,H69B), C69(H69C,H69D), C65(H65A,H65B),
 C86(H86A,H86B), C70(H70A,H70B), C91(H91A,H91B), C92(H92A,H92B), C79(H79A,H79B),
  C72A(H72A,H72B), C77(H77A,H77B), C77(H77C,H77D), C78A(H78A,H78B), C71A(H71A,
 H71B), C78B(H78C,H78D), C72B(H72C,H72D), C71B(H71C,H71D), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C18(H18), C15(H15), C47(H47), C49(H49), C48(H48), C17(H17), C16(H16)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C38(H38A,H38B,
 H38C), C42(H42A,H42B,H42C), C7(H7A,H7B,H7C), C44(H44A,H44B,H44C), C40(H40A,
 H40B,H40C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.694
_oxdiff_exptl_absorpt_empirical_full_min 0.364