Octanuclear zinc phosphates with hitherto unknown cluster architectures: ancillary ligand and solvent assisted structural transformations thereof.
Dar, Aijaz A.; Sen, Saumik; Gupta, Sandeep K.; Patwari, G. Naresh; Murugavel, Ramaswamy; Inorganic chemistry 54 (2015) 9458–9469; doi:10.1021/acs.inorgchem.5b01308

data_4346328
_publ_section_title
;
 Octanuclear zinc phosphates with hitherto unknown cluster architectures:
 ancillary ligand and solvent assisted structural transformations thereof.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9458
_journal_page_last               9469
_journal_paper_doi               10.1021/acs.inorgchem.5b01308
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C64 H112 Br4 O24 P4 S8 Zn4'
_chemical_formula_sum            'C64 H112 Br4 O24 P4 S8 Zn4'
_chemical_formula_weight         2227.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.027(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.221(4)
_cell_length_b                   15.0144(18)
_cell_length_c                   20.073(2)
_cell_measurement_reflns_used    16367
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.5
_cell_volume                     9373.3(19)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69983
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.517
_exptl_absorpt_coefficient_mu    3.027
_exptl_absorpt_correction_T_max  0.5828
_exptl_absorpt_correction_T_min  0.5828
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       cubic
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
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_refine_diff_density_min         -2.507
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         16459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0158P)^2^+79.2421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1326
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_reflns_number_total             16459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01308_si_001.cif
_cod_data_source_block           ajz733
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4346328
_shelx_estimated_absorpt_t_min   0.583
_shelx_estimated_absorpt_t_max   0.583
_shelxl_version_number           2013-3
_shelx_res_checksum              29153
_shelx_hkl_checksum              15774