Crystal structure of a low-temperature (100 K) polymorph of catena-poly[(μ2-4,4′-bipyridine-κ2N,N′)-bis(O,O′-diethyldithiophosphato-κ1S)zinc(II)], C18H28N2O4P2S4Zn
Tan, Yee Seng; Tiekink, Edward R.T.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 233–237; doi:10.1515/ncrs-2019-0594

data_8105068
_publ_section_title
;
 Crystal structure of a low-temperature (100 K) polymorph of
 catena-poly[(\m2-4,4&#x2032;-bipyridine-\k2N,N&#x2032;)-bis(O,O&#x2032;-diethyldithiophosphato-\k1S)zinc(II)],
 C18H28N2O4P2S4Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              233
_journal_page_last               237
_journal_paper_doi               10.1515/ncrs-2019-0594
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C72 H112 N8 O16 P8 S16 Zn4'
_chemical_formula_sum            'C72 H112 N8 O16 P8 S16 Zn4'
_chemical_formula_weight         2367.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.9190(10)
_cell_angle_beta                 78.0500(10)
_cell_angle_gamma                68.1700(10)
_cell_formula_units_Z            2
_cell_length_a                   15.23790(10)
_cell_length_b                   17.3322(2)
_cell_length_c                   21.88290(10)
_cell_measurement_reflns_used    73118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4960
_cell_measurement_theta_min      3.5120
_cell_volume                     5159.97(8)
_computing_cell_refinement       'CrysAlisPro [1]'
_computing_data_collection       'CrysAlisPro [1]'
_computing_data_reduction        'CrysAlisPro [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXT 2014/5 [2]'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2558
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            123255
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.756
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'CrysAlisPro [1]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         18426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+3.6630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17365
_reflns_number_total             18426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0594_suppl.cif
_cod_data_source_block           shelx
_cod_database_code               8105068
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.538