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_2311894
_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) [Co (C5 H2 N2 O4)2 (C10 H8 N2)], 3H2 O'
_chemical_formula_moiety         'C16 H36 N +, C20 H12 Co N6 O8 -, 3(H2 O)'
_chemical_formula_sum            'C36 H54 Co N7 O11'
_chemical_formula_weight         819.79
_chemical_name_systematic
;
Tetra-<i>n</i>-butylammonium
(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')bis(2,4-dioxo-1,2,3,4-\
tetrahydropyrimidin-1-ide-6-carboxylato-\k<i>N</i>^1^)cobalt(III) trihydrate
;
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                88.794(11)
_cell_angle_beta                 103.054(9)
_cell_angle_gamma                88.687(11)
_cell_formula_units_Z            2
_cell_length_a                   13.0155(15)
_cell_length_b                   9.4028(14)
_cell_length_c                   16.2640(17)
_cell_measurement_reflns_used    3865
_cell_measurement_temperature    170.0(10)
_cell_measurement_theta_max      28.862
_cell_measurement_theta_min      4.159
_cell_volume                     1937.8(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg, 1996)'
_computing_publication_material  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      170.0(10)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1521
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25546
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         4.222
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.899
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0882P)^2^+1.4515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                5739
_reflns_number_total             6796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3662sup1.cif
_cod_data_source_block           2e
_cod_database_code               2311894
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.862
_shelx_hkl_checksum              87855
_shelx_res_checksum              99632