A second solvatomorph of poly[[μ~4~-<i>N</i>,<i>N</i>'-(1,3,5-oxadiazinane-3,5-diyl)bis(carbamoylmethanoato)]nickel(II)dipotassium]: crystal structure, Hirshfeld surface analysis and semi-empirical geometry optimization
Plutenko, Maksym O.; Haukka, Matti; Husak, Alina O.; Golenya, Irina A.; Mulloev, Nurullo U.; Acta Crystallographica Section E 77 (2021) 1289–1295; doi:10.1107/S2056989021011774

data_2243969
_publ_section_title
;
 A second solvatomorph of
 poly[[\m~4~-<i>N</i>,<i>N</i>'-(1,3,5-oxadiazinane-3,5-diyl)bis(carbamoylmethanoato)]nickel(II)dipotassium]:
 crystal structure, Hirshfeld surface analysis and semi-empirical geometry
 optimization
;
_journal_coeditor_code           TX2044
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1289
_journal_page_last               1295
_journal_paper_doi               10.1107/S2056989021011774
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[K4 Ni2 (C7 H6 N4 O7)2 (H2 O)3]'
_chemical_formula_moiety         'C14 H18 K4 N8 Ni2 O17'
_chemical_formula_sum            'C14 H18 K4 N8 Ni2 O17'
_chemical_formula_weight         844.18
_chemical_name_systematic
Poly[triaquabis[\m~4~-<i>N</i>,<i>N</i>'-(1,3,5-oxadiazinane-3,5-diyl)bis(carbamoylmethanoato)]dinickel(II)tetrapotassium]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 98.240(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3825(5)
_cell_length_b                   7.7039(3)
_cell_length_c                   17.3078(6)
_cell_measurement_reflns_used    12179
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     2689.70(16)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Bruker, 2008)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2009)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25068
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.447
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_T_max  0.8423
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008)
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       orange
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.0539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                5118
_reflns_number_total             6148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2044sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2689.69(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243969
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.842
_shelx_hkl_checksum              85039
_shelx_res_checksum              33228
_cod_database_fobs_code 2243969