Metal-directed self-assembly of transition metal heterometallascorpionates.
Pastor-Medrano, Jesús; Rodríguez-Raya, Francisco R; Bernabé-Pablo, Erandi; Mireles-Chávez, Daniel A; Jancik, Vojtech; Martínez-Otero, Diego; Moya-Cabrera, Mónica; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6571–6580; doi:10.1039/c9dt00683d

data_7049816
_publ_section_title
;
 Metal-directed self-assembly of transition metal
 heterometallascorpionates.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6571
_journal_page_last               6580
_journal_paper_doi               10.1039/c9dt00683d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C172 H152 Co2 K2 N18 O4 P12 S12, 1.696(C4 H8 O), 0.304(C H2 Cl2)'
_chemical_formula_sum
'C179.09 H166.18 Cl0.61 Co2 K2 N18 O5.7 P12 S12'
_chemical_formula_weight         3635.79
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-01-20 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.6410(10)
_cell_angle_beta                 88.9410(10)
_cell_angle_gamma                62.3750(10)
_cell_formula_units_Z            1
_cell_length_a                   16.0136(4)
_cell_length_b                   16.3827(4)
_cell_length_c                   20.3288(5)
_cell_measurement_reflns_used    9323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.21
_cell_volume                     4288.04(19)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            111939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.463
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2, Sheldrick'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1887
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/THF'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1469
_refine_ls_number_reflns         16862
_refine_ls_number_restraints     2420
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0291P)^2^+4.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15466
_reflns_number_total             16862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00683d2.cif
_cod_data_source_block           Comp3
_cod_depositor_comments
'Adding full bibliography for 7049816--7049826.cif.'
_cod_original_formula_sum
'C179.09 H166.18 Cl0.61 Co2 K2 N18 O5.70 P12 S12'
_cod_database_code               7049816
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              71906