Cobalt complexes of the chelating dicarboxylate ligand "esp": a paddlewheel-type dimer and a heptanuclear coordination cluster.
Pakula, Ryan J.; Berry, John F.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13887–13893; doi:10.1039/c8dt03030h

data_7047380
_publ_section_title
;
 Cobalt complexes of the chelating dicarboxylate ligand &quot;esp&quot;: a
 paddlewheel-type dimer and a heptanuclear coordination cluster.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13887
_journal_page_last               13893
_journal_paper_doi               10.1039/c8dt03030h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C100 H132 Co7 N2 O28, 4(C2 H3 N)'
_chemical_formula_sum            'C108 H144 Co7 N6 O28'
_chemical_formula_weight         2386.79
_chemical_name_systematic        Co7(OH)4(Hesp)2(esp)4(MeCN)2.4MeCN
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                94.052(3)
_cell_angle_beta                 94.507(3)
_cell_angle_gamma                95.506(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4865(8)
_cell_length_b                   17.3169(9)
_cell_length_c                   22.9538(12)
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.279
_cell_measurement_theta_min      2.183
_cell_volume                     5696.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Gromit
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21148
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.443
_diffrn_reflns_theta_min         1.185
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.734107
_exptl_absorpt_correction_T_min  0.506381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 126376 reflections, Rint = 0.0803
 (38835 with I > 3sig(I), Rint = 0.0649)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2494
_exptl_crystal_recrystallization_method 'Grown from MeCN in air'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1387
_refine_ls_number_reflns         21148
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0463P)^2^+12.0007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18621
_reflns_number_total             21148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03030h2.cif
_cod_data_source_block           twin4
_cod_depositor_comments
'Adding full bibliography for 7047379--7047380.cif.'
_cod_database_code               7047380
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8331(5)
 0.1669(5)
2. 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, All O(H) groups
3. Restrained distances
 O1-H1
 0.84 with sigma of 0.02
 O3-H3
 0.84 with sigma of 0.02
 O4-H4
 0.84 with sigma of 0.02
 O2-H2
 0.84 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C16(H16A,H16B), C25(H25A,H25B), C32(H32A,H32B), C41(H41A,H41B),
 C48(H48A,H48B), C57(H57A,H57B), C64(H64A,H64B), C73(H73A,H73B), C80(H80A,H80B),
  C89(H89A,H89B), C96(H96A,H96B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C15(H15), C27(H27), C28(H28), C29(H29),
 C31(H31), C43(H43), C44(H44), C45(H45), C47(H47), C59(H59), C60(H60), C61(H61),
  C63(H63), C75(H75), C76(H76), C77(H77), C79(H79), C91(H91), C92(H92),
 C93(H93), C95(H95)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C2S(H2SA,
 H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,H8SC)
4.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O20(H20)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen mount'
_olex2_submission_original_sample_id Co7
_olex2_submission_special_instructions 'No special instructions were received'