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_7711674
_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         'C60 H114 Co2 K N4 O3 P4'
_chemical_formula_sum            'C60 H114 Co2 K N4 O3 P4'
_chemical_formula_weight         1220.39
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-07-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-31 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.199(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7989(7)
_cell_length_b                   13.3737(3)
_cell_length_c                   22.8232(6)
_cell_measurement_reflns_used    12575
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.2850
_cell_measurement_theta_min      2.2550
_cell_volume                     6732.4(4)
_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      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -26.00  90.00   0.50    7.42    --   12.90  77.00 -60.00  232
  2  \w    -18.00  28.00   0.50    7.42    --   12.90  77.00  30.00   92
  3  \w     62.00 101.00   0.50    7.42    --   12.90  77.00  30.00   78
  4  \w    -71.00   0.00   0.50    7.42    --   12.90 -77.00   0.00  142
  5  \w    -27.00  29.00   0.50    7.42    --   12.90 -57.00-150.00  112
;
_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      -0.0239723000
_diffrn_orient_matrix_UB_12      0.0085275000
_diffrn_orient_matrix_UB_13      -0.0320234000
_diffrn_orient_matrix_UB_21      -0.0016828000
_diffrn_orient_matrix_UB_22      0.0505630000
_diffrn_orient_matrix_UB_23      0.0084435000
_diffrn_orient_matrix_UB_31      0.0213716000
_diffrn_orient_matrix_UB_32      0.0135743000
_diffrn_orient_matrix_UB_33      -0.0111731000
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25916
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         2.006
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57027
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7712
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0703P)^2^+12.9504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6497
_reflns_number_total             7712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03320h2.cif
_cod_data_source_block           exp_9511
_cod_database_code               7711674
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Co O Br'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.863
_reflns_odcompleteness_completeness 99.75
_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
2. Restrained distances
 C29-C30
 1.54 with sigma of 0.02
 O2-C29
 1.45 with sigma of 0.02
 O1A-C25A = O1A-C28A
 1.45 with sigma of 0.02
 C28A-C27A = C26A-C27A = C26A-C25A
 1.54 with sigma of 0.01
 O1-C25 = O1-C28
 1.45 with sigma of 0.02
 C25-C26 = C27-C26 = C27-C28
 1.54 with sigma of 0.01
 O1A-C26A
 2.5 with sigma of 0.04
 O1A-C27A
 2.5 with sigma of 0.04
 C28A-C26A
 2.5 with sigma of 0.04
 C27A-C25A
 2.5 with sigma of 0.04
 C28A-C25A
 2.5 with sigma of 0.04
 O1-C26
 2.5 with sigma of 0.04
 O1-C27
 2.5 with sigma of 0.04
 C25-C28
 2.5 with sigma of 0.04
 C25-C27
 2.5 with sigma of 0.04
 C28-C26
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C29 \\sim C30: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
O2 \\sim C29 \\sim C30: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O1A \\sim C25A \\sim C26A \\sim C27A \\sim C28A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
O1 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C7) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(O1A)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(O1)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28B)=Sof(H28A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1A), C7(H7), C13(H13), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8B,H8A),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C25A(H25C,H25D), C26(H26A,H26B), C26A(H26C,H26D), C27(H27A,H27B),
 C27A(H27C,H27D), C28(H28B,H28A), C28A(H28C,H28D), C29(H29B,H29A), C30(H30A,
 H30B)
;
_shelx_res_checksum              37166
_shelx_hkl_checksum              39890
_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.749