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_7708352
_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         'C49 H77 Co Mg N2 O P4, C7 H8'
_chemical_formula_sum            'C56 H86 Co Mg N2 O P4'
_chemical_formula_weight         1010.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 96.235(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8957(8)
_cell_length_b                   12.5578(4)
_cell_length_c                   41.1155(11)
_cell_measurement_reflns_used    9601
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.3270
_cell_measurement_theta_min      4.4940
_cell_volume                     11238.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.970
_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    -38.00  26.00   1.00   22.50    --   42.04 -19.00-180.00   64
  2  \w    -38.00  16.00   1.00   22.50    --   42.04 -19.00 120.00   54
  3  \w    -13.00  41.00   1.00   22.50    --   42.04 -37.00 -60.00   54
  4  \w     15.00  40.00   1.00   22.50    --   42.04 -37.00 -30.00   25
  5  \w    -36.00  25.00   1.00   22.50    --   42.04 -19.00-120.00   61
  6  \w     88.00 115.00   1.00   75.00    --  104.40  77.00 -60.00   27
  7  \w     88.00 152.00   1.00   75.00    --  104.40  45.00  30.00   64
  8  \w     76.00 137.00   1.00   75.00    --  104.40  30.00 -90.00   61
  9  \w     35.00  63.00   1.00   75.00    --  104.40 -61.00 -30.00   28
 10  \w     32.00  58.00   1.00   75.00    --  104.40 -61.00-180.00   26
 11  \w     32.00  58.00   1.00   75.00    --  104.40 -61.00 150.00   26
 12  \w    130.00 157.00   1.00   75.00    --  104.40  77.00-150.00   27
 13  \w     98.00 158.00   1.00   75.00    --  104.40  77.00 -90.00   60
 14  \w     46.00  87.00   1.00   75.00    --  104.40-125.00  90.00   41
 15  \w    127.00 154.00   1.00   75.00    --  104.40  77.00 -60.00   27
 16  \w     29.00 106.00   1.00   75.00    --  104.40 -77.00 120.00   77
 17  \w     38.00  83.00   1.00   75.00    --  104.40 -77.00 -60.00   45
;
_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      0.0033759000
_diffrn_orient_matrix_UB_12      0.0604788000
_diffrn_orient_matrix_UB_13      -0.0323469000
_diffrn_orient_matrix_UB_21      -0.0666119000
_diffrn_orient_matrix_UB_22      0.0384588000
_diffrn_orient_matrix_UB_23      0.0008917000
_diffrn_orient_matrix_UB_31      0.0237325000
_diffrn_orient_matrix_UB_32      0.0995709000
_diffrn_orient_matrix_UB_33      0.0193080000
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            24615
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.848
_diffrn_reflns_theta_min         3.682
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+14.2694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9567
_reflns_number_total             10888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           jkc35
_cod_database_code               7708352
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H Co Mg N P O'
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.337
_reflns_odcompleteness_completeness 99.47
_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:
 C22(H22a,H22b), C46(H46a,H46b), C24(H24a,H24b), C49(H49a,H49b), C14(H14a,
 H14b), C48(H48a,H48b), C12(H12a,H12b), C47(H47a,H47b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C18(H18), C19(H19), C10(H10), C8(H8), C9(H9), C51(H51),
 C55(H55), C53(H53), C54(H54), C50(H50)
2.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C29(H29a,H29b,H29c), C38(H38a,H38b,H38c), C4(H4a,H4b,H4c),
 C30(H30a,H30b,H30c), C45(H45a,H45b,H45c), C28(H28a,H28b,H28c), C35(H35a,H35b,
 H35c), C23(H23a,H23b,H23c), C33(H33a,H33b,H33c), C40(H40a,H40b,H40c), C25(H25a,
 H25b,H25c), C34(H34a,H34b,H34c), C43(H43a,H43b,H43c), C39(H39a,H39b,H39c),
 C15(H15a,H15b,H15c), C44(H44a,H44b,H44c), C13(H13a,H13b,H13c), C52(H52a,H52b,
 H52c)
;
_shelx_res_checksum              36320
_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 5.366
_oxdiff_exptl_absorpt_empirical_full_min 0.275