Dinitrogen activation by a phosphido-bridged binuclear cobalt complex
Li, Hai-Jun; Feng, Rui; Wang, Gao-Xiang; Wei, Junnian; Xi, Zhenfeng; Dalton Transactions  (2022) –; doi:10.1039/D2DT03320H

data_7711675
_publ_section_title
;
 Dinitrogen activation by a phosphido-bridged binuclear cobalt complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03320H
_journal_year                    2022
_chemical_formula_moiety         'C27 H46 Br Co N P2'
_chemical_formula_sum            'C27 H46 Br Co N P2'
_chemical_formula_weight         585.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-13 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.827(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8615(3)
_cell_length_b                   15.4191(4)
_cell_length_c                   19.5790(5)
_cell_measurement_reflns_used    11907
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.8090
_cell_measurement_theta_min      2.5290
_cell_volume                     2913.89(14)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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    -80.00  63.00   0.50    1.32    --   -9.60   0.00-120.00  286
  2  \w    -52.00  -4.00   0.50    1.32    --   -9.60  82.00 -90.00   96
  3  \w     -6.00  20.00   0.50    1.32    --    9.60  82.00-150.00   52
  4  \w     65.00  96.00   0.50    1.32    --    9.60  82.00-150.00   62
  5  \w     -6.00  74.00   0.50    1.32    --    9.60  38.00-150.00  160
;
_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      -0.0170230000
_diffrn_orient_matrix_UB_12      -0.0380946000
_diffrn_orient_matrix_UB_13      0.0167465000
_diffrn_orient_matrix_UB_21      -0.0253316000
_diffrn_orient_matrix_UB_22      -0.0193461000
_diffrn_orient_matrix_UB_23      -0.0329785000
_diffrn_orient_matrix_UB_31      0.0668802000
_diffrn_orient_matrix_UB_32      -0.0170741000
_diffrn_orient_matrix_UB_33      0.0000816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25300
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.110
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49803
_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            'dull dark green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0306P)^2^+1.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5651
_reflns_number_total             6627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03320h2.cif
_cod_data_source_block           exp_9935
_cod_database_code               7711675
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Co Br O'
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.819
_reflns_odcompleteness_completeness 99.16
_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(C12)=Sof(H12C)=Sof(H12D)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(C11)=Sof(H11C)=Sof(H11D)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1)=Sof(C10)=Sof(H10C)=Sof(H10D)=Sof(C7)=Sof(H7)=
 Sof(P1)=1-FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C1A)=Sof(H1A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C10A)=
 Sof(H10A)=Sof(H10B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(P1A)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C7A(H7A), C1A(H1A), C1(H1), C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C13(H13A,H13B), C20(H20A,H20B), C8A(H8AA,H8AB), C2A(H2AA,
 H2AB), C9A(H9AA,H9AB), C6A(H6AA,H6AB), C11A(H11A,H11B), C12A(H12A,H12B),
 C10A(H10A,H10B), C3A(H3AA,H3AB), C5A(H5AA,H5AB), C4A(H4AA,H4AB), C12(H12C,
 H12D), C8(H8A,H8B), C6(H6A,H6B), C5(H5A,H5B), C2(H2A,H2B), C9(H9A,H9B),
 C11(H11C,H11D), C3(H3A,H3B), C4(H4A,H4B), C10(H10C,H10D)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C18(H18), C17(H17)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              61723
_shelx_hkl_checksum              83271
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.688