Preparation and reactivity of a square-planar PNP cobalt(ii)-hydrido complex: isolation of the first {Co-NO}<sup>8</sup>-hydride.
Krishnan, V. Mahesh; Arman, Hadi D.; Tonzetich, Zachary J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1435–1441; doi:10.1039/c7dt04339b

data_7045039
_publ_section_title
;
 Preparation and reactivity of a square-planar PNP cobalt(ii)-hydrido
 complex: isolation of the first {Co-NO}<sup>8</sup>-hydride.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1435
_journal_page_last               1441
_journal_paper_doi               10.1039/c7dt04339b
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H43 Co N O2 P2'
_chemical_formula_sum            'C23 H43 Co N O2 P2'
_chemical_formula_weight         486.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-15 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.796(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6498(4)
_cell_length_b                   15.2862(5)
_cell_length_c                   15.6734(6)
_cell_measurement_reflns_used    10345
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9770
_cell_measurement_theta_min      2.6180
_cell_volume                     2527.97(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -72.00  80.00   1.00   50.00    --   -9.70  10.00-176.00  152
  2  \w    -85.00  26.00   1.00   50.00    --    4.20 -38.00 -60.00  111
  3  \w    -99.00  20.00   1.00   50.00    --   -9.70 -57.00 -60.00  119
  4  \w    -99.00  15.00   1.00   50.00    --   -9.70 -38.00-150.00  114
  5  \w    -42.00  80.00   1.00   50.00    --   -9.70  72.00   0.00  122
  6  \w    -99.00  20.00   1.00   50.00    --   -9.70 -57.00  60.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489805000
_diffrn_orient_matrix_UB_12      -0.0009148000
_diffrn_orient_matrix_UB_13      -0.0354619000
_diffrn_orient_matrix_UB_21      0.0454784000
_diffrn_orient_matrix_UB_22      0.0062712000
_diffrn_orient_matrix_UB_23      -0.0285671000
_diffrn_orient_matrix_UB_31      0.0071064000
_diffrn_orient_matrix_UB_32      -0.0459982000
_diffrn_orient_matrix_UB_33      -0.0032011000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51235
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 3492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8784
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                8615
_reflns_number_total             8784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04339b2.cif
_cod_data_source_block           1609
_cod_depositor_comments
'Adding full bibliography for 7045037--7045039.cif.'
_cod_database_code               7045039
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Co1N2P2C40H20
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.773
_reflns_odcompleteness_completeness 99.92
_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 Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C28(H28A,H28B), C37(H37A,H37B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C2(H2), C26(H26), C46(H46), C3(H3)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C41(H41A,H41B,
 H41C), C40(H40A,H40B,H40C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C34(H34A,
 H34B,H34C), C43(H43A,H43B,H43C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C18(H18A,
 H18B,H18C), C44(H44A,H44B,H44C), C16(H16A,H16B,H16C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C17(H17A,H17B,
 H17C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C)
;
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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 1.737
_oxdiff_exptl_absorpt_empirical_full_min 0.772