First-row transition metal-pyridine (py)-sulfate [(py)<sub>x</sub>M](SO<sub>4</sub>) complexes (M = Ni, Cu and Zn): crystal field theory in action.
Roy, Mrittika; Pham, Duyen N. K.; Kreider-Mueller, Ava; Golen, James A.; Manke, David R.; Acta crystallographica. Section C, Structural chemistry 74 (2018) 263–268; doi:10.1107/S2053229618001547

data_2311983
_publ_section_title
;
 First-row transition metal-pyridine (py)-sulfate
 [(py)<sub>x</sub>M](SO<sub>4</sub>) complexes (M = Ni, Cu and Zn):
 crystal field theory in action.
;
_journal_coeditor_code           FN3254
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              263
_journal_page_last               268
_journal_paper_doi               10.1107/S2053229618001547
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Zn2 (S O4)2 (C5 H5 N1)6]'
_chemical_formula_moiety         'C30 H30 N6 O8 S2 Zn2'
_chemical_formula_sum            'C30 H30 N6 O8 S2 Zn2'
_chemical_formula_weight         797.46
_chemical_name_systematic
<i>catena</i>-Poly[[tetrakis(pyridine-\k<i>N</i>)zinc(II)]-\m-sulfato-\k^2^<i>O</i>:<i>O</i>'-[bis(pyridine-\k<i>N</i>)zinc(II)]-\m-sulfato-\k^2^<i>O</i>:<i>O</i>']
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.5383(10)
_cell_length_b                   10.5383(10)
_cell_length_c                   26.135(3)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      3.23
_cell_volume                     2513.6(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68074
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.720
_diffrn_reflns_theta_min         3.233
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1240 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.004(3)
_refine_ls_extinction_coef       0.0037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0177
_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^)+(0.0267P)^2^+0.6802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                3039
_reflns_number_total             3183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3254sup1.cif
_cod_data_source_block           UMD1296
_cod_original_cell_volume        2513.5(5)
_cod_database_code               2311983
_shelx_estimated_absorpt_t_min   0.610
_shelx_estimated_absorpt_t_max   0.806
_shelx_hkl_checksum              73737
_shelx_res_checksum              67407
_shelxl_version_number           2014/6