Assembly and Properties of Heterobimetallic CoII/III/CaII Complexes with Aquo and Hydroxo Ligands
David C. Lacy; Young Jun Park; Joseph W. Ziller; Junko Yano; A. S. Borovik; Journal of the American Chemical Society 134 (2012) 17526–17535; doi:10.1021/ja304525n

data_4118788
_publ_section_title
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 Assembly and Properties of Heterobimetallic CoII/III/CaII Complexes with
 Aquo and Hydroxo Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17526
_journal_page_last               17535
_journal_paper_doi               10.1021/ja304525n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C44 H69 Ca Co F3 N4 O16 S4'
_chemical_formula_weight         1194.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                73.4591(4)
_cell_angle_beta                 88.5336(4)
_cell_angle_gamma                85.2907(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4438(4)
_cell_length_b                   17.4810(7)
_cell_length_c                   17.5309(7)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.38
_cell_volume                     2765.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33604
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       rod
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
There were several high residuals present in the final difference-Fourier map.
It was not possible to determine the nature of the residuals although it is 
probable that dichloromethane solvent was present.   
;
_refine_diff_density_max         2.350
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         13265
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+2.4148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                11313
_reflns_number_total             13265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304525n_si_003.cif
_cod_data_source_block           asb228
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               4118788