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_7047379
_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         '2(C18 H26 Co O5)'
_chemical_formula_sum            'C36 H52 Co2 O10'
_chemical_formula_weight         762.63
_chemical_name_systematic        Co2(esp)2(EtOH)2
_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             2013-09-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.08.21 svn.r2771 for OlexSys, GUI svn.r4586)
;
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                115.783(2)
_cell_angle_beta                 91.404(2)
_cell_angle_gamma                114.197(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0937(5)
_cell_length_b                   13.2312(6)
_cell_length_c                   14.6240(6)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.66
_cell_measurement_theta_min      3.46
_cell_volume                     1862.47(15)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\ \w and 0.6\ \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6780
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.025
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.421
_exptl_absorpt_correction_T_max  0.151491
_exptl_absorpt_correction_T_min  0.031307
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1267 before and 0.0520 after correction.
 The Ratio of minimum to maximum transmission is 0.21.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1273 before and 0.0515 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 53595 reflections, Rint = 0.0511
 (42350 with I > 3sig(I), Rint = 0.0494)
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_recrystallization_method
'Grown by slow evaporation of an EtOH solution of the complex at room temperature in air.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0753P)^2^+0.2165P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6359
_reflns_number_total             6780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03030h2.cif
_cod_data_source_block           berry236
_cod_depositor_comments
'Adding full bibliography for 7047379--7047380.cif.'
_cod_original_cell_volume        1862.46(14)
_cod_database_code               7047379
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.155
_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, All O(H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 O10A-H10A
 0.87 with sigma of 0.01
 C17-H5
 1.90546 with sigma of 0.02
 Co1-H5
 2.647093 with sigma of 0.02
 C35-H10
 1.900594 with sigma of 0.02
 Co2-H10
 2.59407 with sigma of 0.02
 C35A-H10A
 2.009091 with sigma of 0.02
 Co2-H10A
 2.758604 with sigma of 0.02
3. Others
 Sof(O10A)=Sof(H10A)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(O10)=Sof(H10)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C17(H17A,H17B), C23(H23A,H23B), C30(H30A,H30B),
 C35(H35A,H35B), C35A(H35C,H35D)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C11(H11), C25(H25), C26(H26), C27(H27), C29(H29)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              4161