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_7045037
_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_formula_moiety         'C22 H46 B Co N P2'
_chemical_formula_sum            'C22 H46 B Co N P2'
_chemical_formula_weight         456.28
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-09-26
_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                 112.919(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2602(10)
_cell_length_b                   11.3904(6)
_cell_length_c                   15.6393(12)
_cell_measurement_reflns_used    5616
_cell_measurement_temperature    98
_cell_measurement_theta_max      27.3250
_cell_measurement_theta_min      2.9480
_cell_volume                     2503.8(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      98
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -99.00  15.00   1.00   55.00    --   -9.70 -38.00-120.00  114
  2  \w    -99.00  15.00   1.00   55.00    --   -9.70 -38.00   0.00  114
  3  \w    -99.00  20.00   1.00   55.00    --   -9.70 -57.00   0.00  119
  4  \w    -34.00  11.00   1.00   55.00    --   -9.70  38.00   0.00   45
;
_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      0.0107635000
_diffrn_orient_matrix_UB_12      0.0604583000
_diffrn_orient_matrix_UB_13      -0.0007866000
_diffrn_orient_matrix_UB_21      0.0152650000
_diffrn_orient_matrix_UB_22      0.0023433000
_diffrn_orient_matrix_UB_23      0.0490129000
_diffrn_orient_matrix_UB_31      0.0468798000
_diffrn_orient_matrix_UB_32      -0.0146293000
_diffrn_orient_matrix_UB_33      0.0048699000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.550
_diffrn_reflns_theta_max         24.550
_diffrn_reflns_theta_min         2.279
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75448
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0100P)^2^+26.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4100
_reflns_number_total             4185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04339b2.cif
_cod_data_source_block           cd1603
_cod_depositor_comments
'Adding full bibliography for 7045037--7045039.cif.'
_cod_database_code               7045037
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.735
_reflns_odcompleteness_completeness 99.93
_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, All C(H,H,H,H,H,H,H) groups
2. Restrained distances
 C21B-C19
 1.45 with sigma of 0.02
 C16A-C15
 1.45 with sigma of 0.02
 C9A-C6A
 1.45 with sigma of 0.02
 C6B-P1
 1.8 with sigma of 0.02
 C17B-C15
 1.5 with sigma of 0.02
 C17A-C15
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6B) = Uanis(C9A) = Uanis(C9B) = Uanis(C8B) = Uanis(C8A) = Uanis(C6A) =
Uanis(C7A) = Uanis(C7B)
Uanis(C15) = Uanis(C17A) = Uanis(C17B) = Uanis(C18B) = Uanis(C18A) =
Uanis(C16A) = Uanis(C16B)
Uanis(C22B) = Uanis(C22A) = Uanis(C19) = Uanis(C21A) = Uanis(C21B) =
Uanis(C20B) = Uanis(C20A)
Uanis(C12B) = Uanis(C12A) = Uanis(C10) = Uanis(C13B) = Uanis(C13A) =
Uanis(C3BA) = Uanis(C11A) = Uanis(C11B)
Uanis(C5) = Uanis(C1) = Uanis(N1) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(C14A) = Uanis(C14B)
4. Others
 Fixed Sof: C21B(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C16B(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C17B(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18A(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C22A(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
 C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5)
 C6B(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5)
 H8BC(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C6A(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) H9AC(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C16A(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5) C18B(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C17A(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
 C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C20A(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5) C12A(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C10(0.5) C13A(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C11B(0.5)
 H11D(0.5) H11E(0.5) H11F(0.5) C12B(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 C3BA(0.5) C13B(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C14A(0.5) H14A(0.5)
 H14B(0.5) C14B(0.5) H14C(0.5) H14D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C14A(H14A,H14B), C14B(H14C,H14D)
5.b Me refined as rotating group:
 C9B(H9BA,H9BB,H9BC), C9A(H9AA,H9AB,H9AC)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
5.d Idealised Me refined as rotating group:
 C21B(H21A,H21B,H21C), C16B(H16A,H16B,H16C), C17B(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C22A(H22A,H22B,H22C), C20B(H20A,H20B,H20C), C7B(H7BA,H7BB,H7BC),
 C8B(H8BA,H8BB,H8BC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C16A(H16D,H16E,
 H16F), C18B(H18D,H18E,H18F), C17A(H17D,H17E,H17F), C21A(H21D,H21E,H21F),
 C22B(H22D,H22E,H22F), C20A(H20D,H20E,H20F), C12A(H12A,H12B,H12C), C13A(H13A,
 H13B,H13C), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F),
 C13B(H13D,H13E,H13F)
;
_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 1.679
_oxdiff_exptl_absorpt_empirical_full_min 0.720