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_7706968
_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            'C22 H26 Co I N3 O2'
_chemical_formula_weight         550.29
_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_rem7a
_audit_creation_date             2020-05-29
_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                 102.3353(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.83518(11)
_cell_length_b                   11.45668(12)
_cell_length_c                   16.88113(15)
_cell_measurement_reflns_used    50128
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      34.1110
_cell_measurement_theta_min      2.7070
_cell_volume                     2236.10(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_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 0.979
_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      5.00 103.00   0.50   15.00    --   30.66  38.00  90.00  196
  2  \w    -20.00  73.00   0.50   15.00    --   30.66 -99.00 150.00  186
  3  \w      1.00 101.00   0.50   15.00    --   30.66  77.00-150.00  200
  4  \w    -20.00  73.00   0.50   15.00    --   30.66 -99.00 -90.00  186
  5  \w     10.00  99.00   0.50   15.00    --   30.66  57.00 -30.00  178
  6  \w     10.00  99.00   0.50   15.00    --   30.66  57.00 120.00  178
  7  \w    -20.00  73.00   0.50   15.00    --   30.66 -99.00  90.00  186
  8  \w    -38.00  52.00   0.50   15.00    --   30.66 -57.00-180.00  180
  9  \w      1.00 101.00   0.50   15.00    --   30.66  77.00 150.00  200
 10  \w      1.00 101.00   0.50   15.00    --   30.66  77.00   0.00  200
 11  \w      1.00 101.00   0.50   15.00    --   30.66  77.00 -90.00  200
 12  \w    -20.00  73.00   0.50   15.00    --   30.66 -99.00 -30.00  186
 13  \w      1.00 101.00   0.50   15.00    --   30.66  77.00  90.00  200
 14  \w      5.00 103.00   0.50   15.00    --   30.66  38.00 -90.00  196
 15  \w    -38.00  52.00   0.50   15.00    --   30.66 -57.00 120.00  180
 16  \w    -42.00  56.00   0.50   15.00    --   30.66 -38.00 -60.00  196
 17  \f      0.00 120.00   0.50   15.00  31.58  30.66 -40.00    --   240
 18  \f      0.00 120.00   0.50   15.00  29.73  30.66  40.00    --   240
 19  \f      0.00  27.00   0.50   15.00  78.88  30.66  40.00    --    54
 20  \f      0.00 120.00   0.50   15.00 -17.57  30.66 -40.00    --   240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0563163000
_diffrn_orient_matrix_UB_12      0.0123892000
_diffrn_orient_matrix_UB_13      0.0228052000
_diffrn_orient_matrix_UB_21      0.0234265000
_diffrn_orient_matrix_UB_22      -0.0132300000
_diffrn_orient_matrix_UB_23      -0.0342812000
_diffrn_orient_matrix_UB_31      -0.0066123000
_diffrn_orient_matrix_UB_32      0.0591931000
_diffrn_orient_matrix_UB_33      -0.0124336000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            120221
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.249
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 7058 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         17938
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0196P)^2^+0.2777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                16530
_reflns_number_total             17938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00277e2.cif
_cod_data_source_block           ga_rem7a
_cod_depositor_comments
'Adding full bibliography for 7706966--7706972.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7706968
_audit_block_refno               3568
_audit_block_usercomment         'rm40 dark red block'
_reflns_odcompleteness_completeness 99.95
_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), C51(H51), C66(H66), C67(H67), C70(H70)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C52(H52A,H52B), C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C54(H54), C57(H57),
 C58(H58), C59(H59), C60(H60), C63(H63)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.840
_shelx_res_checksum              18116