Tetraaqua[3-oxo-1,3-bis(pyridinium-2-yl)propan-1-olato]nickel(II) tribromide dihydrate
Westcott, Barry L.; Crundwell, Guy; Alicea-Velázquez, Nilda L.; Acta Crystallographica Section E 76 (2020) 270–272; doi:10.1107/S205698902000081X

data_2243264
_publ_section_title
;
 Tetraaqua[3-oxo-1,3-bis(pyridinium-2-yl)propan-1-olato]nickel(II)
 tribromide dihydrate
;
_journal_coeditor_code           ZL2768
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              270
_journal_page_last               272
_journal_paper_doi               10.1107/S205698902000081X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ni (C13 H11 N2 O2) (H2 O1)4] 3Br, 2H2 O'
_chemical_formula_moiety         'C13 H19 N2 Ni O6 3+, 3(Br -), 2(H2 O)'
_chemical_formula_sum            'C13 H23 Br3 N2 Ni O8'
_chemical_formula_weight         633.77
_chemical_name_systematic
;
Tetraaqua[3-oxo-1,3-bis(pyridinium-2-yl)propan-1-olato]nickel(II) tribromide
dihydrate
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.00
_cell_angle_beta                 97.476(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8071(6)
_cell_length_b                   23.8031(16)
_cell_length_c                   13.6302(10)
_cell_measurement_reflns_used    4741
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0640
_cell_measurement_theta_min      4.5660
_cell_volume                     2189.7(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED  (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
OLEX2 (Bourhis <i>et al.</i>,  2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1790
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26929
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         33.715
_diffrn_reflns_theta_min         4.333
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7970
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0561P)^2^+2.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                5803
_reflns_number_total             7970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2768sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243264
_cod_database_fobs_code          2243264
_shelx_hkl_checksum              31969
_shelx_res_checksum              12760