Low-oxidation state cobalt‒magnesium complexes: ion-pairing and reactivity
Kelly, John A.; Gramüller, Johannes; Gschwind, Ruth M.; Wolf, Robert; Dalton Transactions  (2021) –; doi:10.1039/D1DT02621F

data_7708349
_publ_section_title
;
 Low-oxidation state cobalt--magnesium complexes: ion-pairing and
 reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02621F
_journal_year                    2021
_chemical_formula_moiety         'C39 H53 Co Mg N2'
_chemical_formula_sum            'C39 H53 Co Mg N2'
_chemical_formula_weight         633.07
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.952(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0053(4)
_cell_length_b                   15.5613(3)
_cell_length_c                   14.1623(3)
_cell_measurement_reflns_used    11969
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.1540
_cell_measurement_theta_min      4.0920
_cell_volume                     3266.64(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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     16.00 113.00   1.00    3.00    --   42.56  57.00 150.00   97
  2  \w     20.00 115.00   1.00    3.00    --   42.56  37.00 -90.00   95
  3  \w      2.00  98.00   1.00    3.00    --   42.56-125.00 120.00   96
  4  \w    -20.00  82.00   1.00    3.00    --   42.56 -99.00  30.00  102
  5  \w     36.00  69.00   1.00   10.00    --  111.00 -30.00  90.00   33
  6  \w     36.00  69.00   1.00   10.00    --  111.00 -30.00 120.00   33
  7  \w     36.00  69.00   1.00   10.00    --  111.00 -30.00  60.00   33
  8  \w     83.00 158.00   1.00   10.00    --  111.00  61.00  30.00   75
  9  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00 -30.00   79
 10  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00  60.00   79
 11  \w     80.00 158.00   1.00   10.00    --  111.00  77.00  90.00   78
 12  \w     39.00 121.00   1.00   10.00    --  111.00-125.00 -60.00   82
 13  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00-150.00   79
 14  \w     39.00 121.00   1.00   10.00    --  111.00-125.00-150.00   82
 15  \w     36.00  69.00   1.00   10.00    --  111.00 -30.00  30.00   33
 16  \w     31.00 156.00   1.00   10.00    --  111.00 -15.00 -60.00  125
 17  \w     40.00  77.00   1.00   10.00    --  111.00 -45.00-180.00   37
 18  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00 120.00   79
 19  \w     11.00 116.00   1.00    3.00    --   42.56  77.00   0.00  105
 20  \w     11.00 116.00   1.00    3.00    --   42.56  77.00  90.00  105
 21  \w    -30.00  65.00   1.00    3.00    --   42.56 -37.00-150.00   95
 22  \w     11.00 116.00   1.00    3.00    --   42.56  77.00-150.00  105
 23  \w     11.00 116.00   1.00    3.00    --   42.56  77.00 -60.00  105
 24  \w     87.00 158.00   1.00   10.00    --  111.00  30.00 -30.00   71
 25  \w     87.00 158.00   1.00   10.00    --  111.00  45.00 150.00   71
 26  \w     80.00 136.00   1.00   10.00    --  111.00  77.00  60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0963825000
_diffrn_orient_matrix_UB_12      -0.0315509000
_diffrn_orient_matrix_UB_13      0.0053428000
_diffrn_orient_matrix_UB_21      -0.0346046000
_diffrn_orient_matrix_UB_22      0.0932583000
_diffrn_orient_matrix_UB_23      -0.0103684000
_diffrn_orient_matrix_UB_31      -0.0177836000
_diffrn_orient_matrix_UB_32      -0.0104016000
_diffrn_orient_matrix_UB_33      -0.1095124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.442
_diffrn_reflns_theta_min         4.119
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0553P)^2^+2.6778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3324
_reflns_number_total             3389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           jkc1_mc_first_try
_cod_database_code               7708349
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C39 H53 Co Mg N2 '
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.287
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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:
 C13(H13), C18(H18), C17(H17), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C20(H20a,H20b), C16(H16a,H16b), C15(H15a,H15b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C6(H6)
2.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C3(H3a,H3b,H3c), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              62621
_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 3.422
_oxdiff_exptl_absorpt_empirical_full_min 0.477