A cuboidal [Cu~4~(SO~4~)~4~] structure supported by β-picoline ligands
Park, Ava M.; Golen, James A.; Manke, David R.; Acta Crystallographica Section E 78 (2022) 108–110; doi:10.1107/S2056989022000780

data_2244022
_publ_section_title
;
 A cuboidal [Cu~4~(SO~4~)~4~] structure supported by \b-picoline ligands
;
_journal_coeditor_code           ZL5027
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              108
_journal_page_last               110
_journal_paper_doi               10.1107/S2056989022000780
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Co4 (S O4)4 (C6 H7 N)8]'
_chemical_formula_moiety         'C48 H56 Co4 N8 O16 S4'
_chemical_formula_sum            'C48 H56 Co4 N8 O16 S4'
_chemical_formula_weight         1364.96
_chemical_name_systematic
;
Tetra-\m~3~-sulfato-tetrakis[bis(3-methylpyridine)cobalt(II)]
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6121(16)
_cell_length_b                   15.6121(16)
_cell_length_c                   11.8359(13)
_cell_measurement_reflns_used    9496
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.92
_cell_volume                     2884.9(5)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54595
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         2.917
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2018)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.201
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1117 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       0.0049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0190
_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^)+(0.0165P)^2^+1.2064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                2624
_reflns_number_total             2744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5027sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2884.9(7)
_cod_database_code               2244022
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.774
_shelx_hkl_checksum              16438
_shelx_res_checksum              27628
_cod_database_fobs_code 2244022