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_7708354
_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         'C35 H51 Co Mg N2 P6'
_chemical_formula_sum            'C35 H51 Co Mg N2 P6'
_chemical_formula_weight         768.83
_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             2021-01-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-08 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9829(2)
_cell_length_b                   18.9262(2)
_cell_length_c                   16.1632(2)
_cell_measurement_reflns_used    22309
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.8480
_cell_measurement_theta_min      4.1340
_cell_volume                     7566.04(14)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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    -67.00  32.00   1.00    4.13    --  -42.29  37.00  60.00   99
  2  \w    -75.00  34.00   1.00    4.13    --  -42.29  77.00 -60.00  109
  3  \w     24.00 109.00   1.00   16.52    --  106.40 -94.00  90.00   85
  4  \w     30.00  69.00   1.00   16.52    --  106.40 -30.00 150.00   39
  5  \w     81.00 158.00   1.00   16.52    --  106.40  45.00  30.00   77
  6  \w     30.00  69.00   1.00   16.52    --  106.40 -30.00  30.00   39
  7  \w     73.00 158.00   1.00   16.52    --  106.40 125.00-120.00   85
  8  \w     30.00  69.00   1.00   16.52    --  106.40 -30.00 120.00   39
  9  \w     82.00 158.00   1.00   16.52    --  106.40  38.00 -36.00   76
 10  \w     73.00 158.00   1.00   16.52    --  106.40 125.00-180.00   85
 11  \w     30.00  69.00   1.00   16.52    --  106.40 -30.00  90.00   39
 12  \w     54.00 158.00   1.00   16.52    --  106.40  15.00 -60.00  104
 13  \w   -114.00 -14.00   1.00    4.13    --  -42.29 -57.00  90.00  100
 14  \w   -118.00 -10.00   1.00    4.13    --  -42.29 -77.00 -30.00  108
 15  \w     54.00 158.00   1.00   16.52    --  106.40  15.00-180.00  104
 16  \w     33.00  77.00   1.00   16.52    --  106.40 -45.00 -90.00   44
 17  \w     33.00 121.00   1.00   16.52    --  106.40-125.00  60.00   88
 18  \w     74.00 158.00   1.00   16.52    --  106.40  77.00  60.00   84
 19  \w     24.00 109.00   1.00   16.52    --  106.40 -94.00-120.00   85
 20  \w     33.00  77.00   1.00   16.52    --  106.40 -45.00-150.00   44
 21  \w   -114.00 -28.00   1.00    4.13    --  -42.29 -57.00-150.00   86
;
_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      -0.0601933000
_diffrn_orient_matrix_UB_12      -0.0159709000
_diffrn_orient_matrix_UB_13      -0.0289910000
_diffrn_orient_matrix_UB_21      0.0148718000
_diffrn_orient_matrix_UB_22      -0.0360470000
_diffrn_orient_matrix_UB_23      -0.0791660000
_diffrn_orient_matrix_UB_31      0.0059101000
_diffrn_orient_matrix_UB_32      -0.0711673000
_diffrn_orient_matrix_UB_33      0.0465813000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.968
_diffrn_reflns_theta_min         3.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0402P)^2^+6.4855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7445
_reflns_number_total             7610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           c2m
_cod_database_code               7708354
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C280 H408 Co8 N16 P56 Mg'
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.186
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C12(H12a,H12b), C24(H24a,H24b), C14(H14a,H14b), C22(H22a,H22b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C10(H10), C20(H20), C9(H9), C19(H19), C18(H18)
2.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C33(H33a,H33b,
 H33c), C5(H5a,H5b,H5c), C25(H25a,H25b,H25c), C13(H13a,H13b,H13c), C29(H29a,
 H29b,H29c), C15(H15a,H15b,H15c), C30(H30a,H30b,H30c), C28(H28a,H28b,H28c),
 C23(H23a,H23b,H23c)
;
_shelx_res_checksum              9302
_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 1.429
_oxdiff_exptl_absorpt_empirical_full_min 0.756