Synthesis and crystal structure of diaquabis(hexamethylenetramine-κ<i>N</i>)bis(thiocyanato-κ<i>N</i>)cobalt(II)–hexamethylenetetramine–acetonitrile (1/2/2)
Krebs, Christoph; Ceglarska, Magdalena; Näther, Christian; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021010033

data_2243939
_publ_section_title
;
 Synthesis and crystal structure of
 diaquabis(hexamethylenetramine-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)--hexamethylenetetramine--acetonitrile
 (1/2/2)
;
_journal_coeditor_code           HB7982
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021010033
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Co (N C S)2 (C6 H12 N4)2 (H2 O1)2], 2C6 H12 N4, 2C2 H3 N'
_chemical_formula_moiety
'C14 H28 Co N10 O2 S2, 2(C6 H12 N4), 2(C2 H3 N)'
_chemical_formula_sum            'C30 H58 Co N20 O2 S2'
_chemical_formula_weight         854.01
_chemical_name_systematic
'Diaquabis(hexamethylenetramine-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)--hexamethylenetetramine--acetonitrile (1/2/2)'
_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     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.899(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0008(2)
_cell_length_b                   12.5903(2)
_cell_length_c                   12.9988(2)
_cell_measurement_reflns_used    20611
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.9120
_cell_measurement_theta_min      3.7290
_cell_volume                     1929.93(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25388
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.044
_diffrn_reflns_theta_min         3.748
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       needle
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0427P)^2^+0.5759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3972
_reflns_number_total             4088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7982sup1.cif
_cod_data_source_block           I
_cod_database_code               2243939
_shelx_hkl_checksum              5452
_shelx_res_checksum              3794
_cod_database_fobs_code 2243939