A phase transition caught in mid-course: independent and concomitant analyses of the monoclinic and triclinic structures of (<sup>n</sup>Bu<sub>4</sub>N)[Co(orotate)<sub>2</sub>(bipy)]·3H<sub>2</sub>O.
Castro, Miguel; Falvello, Larry R.; Forcén-Vázquez, Elena; Guerra, Pablo; Al-Kenany, Nuha A; Martínez, Gema; Tomás, Milagros; Acta crystallographica. Section C, Structural chemistry 73 (2017) 731–742; doi:10.1107/S2053229617010841

data_2311889
_publ_section_title
;
 A phase transition caught in mid-course: independent and concomitant
 analyses of the monoclinic and triclinic structures of
 (<sup>n</sup>Bu<sub>4</sub>N)[Co(orotate)<sub>2</sub>(bipy)]&#x00B7;3H<sub>2</sub>O.
;
_journal_coeditor_code           SK3662
_journal_issue                   'Pt 9'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              731
_journal_page_last               742
_journal_paper_doi               10.1107/S2053229617010841
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'(C16 H36 N)2 [Co (C5 H2 N2 O4)2 (H2 O1)2], 1.8H2 O'
_chemical_formula_moiety
'2(C16 H36 N +), C10 H8 Co N4 O10 2-, 1.8(H2 O)'
_chemical_formula_sum            'C42 H83.6 Co N6 O11.8'
_chemical_formula_weight         920.47
_chemical_name_systematic
;Bis(tetra-<i>n</i>-butylammonium)
diaquabis(2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ide-6-carboxylato-\k<i>N</i>^1^)cobalt(II) 1.8-hydrate
;
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                89.948(3)
_cell_angle_beta                 95.460(3)
_cell_angle_gamma                96.455(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3630(4)
_cell_length_b                   12.6281(5)
_cell_length_c                   16.3765(6)
_cell_measurement_reflns_used    6999
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.7890
_cell_measurement_theta_min      3.0059
_cell_volume                     2528.86(16)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg, 2006)
;
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'four-circle CCD diffractometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26453
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.808
_diffrn_reflns_theta_min         2.994
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  1.0604
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         11477
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                5630
_reflns_number_total             11477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3662sup1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C42 H83.60 Co N6 O11.80'
_cod_database_code               2311889
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.921
_shelx_hkl_checksum              22967
_shelx_res_checksum              11380