Reactivity of a T-shaped cobalt(I) pincer-complex.
Matveeva, Regina; Blasius, Clemens K.; Wadepohl, Hubert; Gade, Lutz H.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6802–6810; doi:10.1039/d1dt00277e

data_7706971
_publ_section_title
;
 Reactivity of a T-shaped cobalt(I) pincer-complex.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6802
_journal_page_last               6810
_journal_paper_doi               10.1039/d1dt00277e
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C30 H30 Co F N3 O2'
_chemical_formula_weight         542.50
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_cbl26
_audit_creation_date             2019-10-01
_audit_creation_method
;
encif (version 1.124)

encifer (version_id = 274361.64)

Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-14 deposited with the CCDC.	2021-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.4658(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2841(2)
_cell_length_b                   6.01267(11)
_cell_length_c                   17.8300(3)
_cell_measurement_reflns_used    13342
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.7090
_cell_measurement_theta_min      3.0990
_cell_volume                     1295.02(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_publication_material
'encif (Wadepohl, 2009-20); encifer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-20xx (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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    -55.00  21.00   0.50   15.00    --  -25.00  77.00  90.00  152
  2  \w     -5.00  21.00   0.50   15.00    --   28.00  82.00  88.84   52
  3  \w     -5.00  21.00   0.50   15.00    --   28.00  82.00-169.61   52
  4  \w     -5.00  21.00   0.50   15.00    --   28.00  82.00 -12.98   52
  5  \w      4.00  93.00   0.50   15.00    --   31.15  72.00 -47.61  178
  6  \w     11.00  52.00   0.50   15.00    --   31.15  57.00 -90.00   82
  7  \w    -38.00  28.00   0.50   15.00    --   31.15 -57.00 120.00  132
  8  \w    -14.00  54.00   0.50   15.00    --   31.15 -99.00-150.00  136
  9  \w    -15.00  65.00   0.50   15.00    --   31.15 -99.00   0.00  160
 10  \w    -37.00  56.00   0.50   15.00    --   31.15 -38.00   0.00  186
 11  \w      5.00  46.00   0.50   15.00    --   31.15  71.00  89.85   82
 12  \w      6.00  97.00   0.50   15.00    --   31.15  38.00 150.00  182
 13  \w      5.00  99.00   0.50   15.00    --   31.15  72.00   7.77  188
 14  \w     40.00  72.00   0.50   15.00    --   31.15 -99.00-120.00   64
 15  \w     65.00  91.00   0.50   15.00    --   31.15  72.00-135.20   52
 16  \w      4.00  41.00   0.50   15.00    --   31.15  72.00-135.20   74
 17  \w     62.00 100.00   0.50   15.00    --   31.15  57.00 -90.00   76
 18  \w     11.00  98.00   0.50   15.00    --   31.15  38.00   0.00  174
 19  \w     17.00  58.00   0.50   15.00    --   31.15  67.00 150.46   82
 20  \w     73.00  99.00   0.50   15.00    --   31.15  67.00 150.46   52
 21  \w     28.00  73.00   0.50   15.00    --   31.15 -99.00  90.00   90
 22  \w    -31.00  56.00   0.50   15.00    --   31.15 -38.00-150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0506514000
_diffrn_orient_matrix_UB_12      0.0012360000
_diffrn_orient_matrix_UB_13      -0.0264546000
_diffrn_orient_matrix_UB_21      -0.0049813000
_diffrn_orient_matrix_UB_22      -0.1166114000
_diffrn_orient_matrix_UB_23      0.0042955000
_diffrn_orient_matrix_UB_31      -0.0293064000
_diffrn_orient_matrix_UB_32      0.0176668000
_diffrn_orient_matrix_UB_33      0.0302967000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.162
_diffrn_reflns_theta_min         2.214
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 3394 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         10195
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0287P)^2^+0.2070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                8776
_reflns_number_total             10195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00277e2.cif
_cod_data_source_block           ga_cbl26
_cod_depositor_comments
'Adding full bibliography for 7706966--7706972.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7706971
_audit_block_refno               3427
_audit_block_usercomment         'CB551, plate, black'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_shelxl_version_number           2018/3
_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 Ternary CH refined with riding coordinates:
 C1(H1), C16(H16), C17(H17), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C26(H26), C27(H27),
 C29(H29), C30(H30)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.265
_oxdiff_exptl_absorpt_empirical_full_min 0.808
_shelx_res_checksum              81735