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_7049819
_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 K2 N18 Ni2 O4 P12 S12, 1.784(C4 H8 O), 0.216(C H2 Cl2)'
_chemical_formula_sum
'C179.35 H166.7 Cl0.43 K2 N18 Ni2 O5.78 P12 S12'
_chemical_formula_weight         3633.86
_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                67.523(1)
_cell_angle_beta                 89.428(1)
_cell_angle_gamma                62.557(1)
_cell_formula_units_Z            1
_cell_length_a                   15.9889(6)
_cell_length_b                   16.2392(6)
_cell_length_c                   20.4481(7)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.20
_cell_volume                     4263.5(3)
_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 0.997
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_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            117974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.764
_diffrn_reflns_theta_min         1.101
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2, Sheldrick'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1888
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/THF'
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.181
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         18120
_refine_ls_number_restraints     5035
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0277P)^2^+7.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15974
_reflns_number_total             18120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00683d2.cif
_cod_data_source_block           Comp5
_cod_depositor_comments
'Adding full bibliography for 7049816--7049826.cif.'
_cod_original_formula_sum
'C179.35 H166.70 Cl0.43 K2 N18 Ni2 O5.78 P12 S12'
_cod_database_code               7049819
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              99108