Synthesis, crystal structure, and characterization of cyclohexylammonium tetraisothiocyanatocobaltate(II): A single-source precursor for cobalt sulfide and oxide nanostructures
A. A. Bagabasa; M. Alsawalha; M. Sohail; S. Alhoshan; R. Arasheed; Heliyon 5 (2019) e01139–; doi:10.1016/j.heliyon.2019.e01139

data_1551111
_publ_section_title
;
 Synthesis, crystal structure, and characterization of cyclohexylammonium
 tetraisothiocyanatocobaltate(II): A single-source precursor for cobalt
 sulfide and oxide nanostructures
;
_journal_name_full               Heliyon
_journal_page_first              e01139
_journal_paper_doi               10.1016/j.heliyon.2019.e01139
_journal_volume                  5
_journal_year                    2019
_chemical_formula_moiety         'C4 Co N4 S4, 2(C6 H14 N)'
_chemical_formula_sum            'C16 H28 Co N6 S4'
_chemical_formula_weight         491.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5881(3)
_cell_length_b                   24.4244(8)
_cell_length_c                   11.4808(4)
_cell_measurement_temperature    130(2)
_cell_volume                     2408.20(14)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
Diamond - Crystal and Molecular Structure Visualization
Crystal Impact - Dr. H. Putz & Dr. K. Brandenburg GbR, Kreuzherrenstr. 
102, 53227 Bonn, Germany
http://www.crystalimpact.com/diamond
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.631
_diffrn_reflns_theta_min         3.619
_exptl_absorpt_coefficient_mu    8.932
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 - Bruker AXS, Madison WI'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       Block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2601
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0733P)^2^+3.3429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2346
_reflns_number_total             2601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
hly_1139_spl_HCHA_spl_2_spl_Co_spl_NCS_spl_4_spl__a.cif
_cod_data_source_block           1
_cod_database_code               1551111
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.414
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B,H5C} of N5, All C(H,H) groups
 At 1.5 times of:
  {H4A,H4B,H4C} of N4
2. Shared sites
{C11A, C11B}
{C8B, C8A}
3. Restrained distances
 C10B-C11A
 1.54 with sigma of 0.01
 C11B-C10A
 1.54 with sigma of 0.01
 C8A-C10B
 2.52 with sigma of 0.02
 C8B-C10A
 2.52 with sigma of 0.02
 C11A-C10B
 1.54 with sigma of 0.01
 C8A-C9A
 1.54 with sigma of 0.01
 C8A-C9A
 1.54 with sigma of 0.01
 C9A-C10A
 1.54 with sigma of 0.01
 C9A-C11A
 2.52 with sigma of 0.02
 C9B-C8B
 1.54 with sigma of 0.01
 C9B-C10B
 1.54 with sigma of 0.01
 C11B-C9B
 2.52 with sigma of 0.02
 C8B-C9B
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C8B) = Uanis(C8A)
Uanis(C11B) = Uanis(C11A)
Uanis(C10A) = Uanis(C10B) = Uanis(C9B) = Uanis(C9A)
5. Rigid body (RIGU) restrains
 C8B, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8B, C8A, C9B, C9A, C10A, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) C8B(0.25) H8A(0.25) N4(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5) S0AA(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) C10A(0.5) H10A(0.5) H10B(0.5) C10B(0.5) H10C(0.5) H10D(0.5)
 C11A(0.25) H11B(0.25) H11C(0.25) C11B(0.25) H11A(0.25) H11D(0.25) C8A(0.25)
 H8B(0.25)
7.a Riding coordinates:
 N5(H5A,H5B,H5C)
7.b Ternary CH refined with riding coordinates:
 C4(H4), C8B(H8A), C8A(H8B)
7.c Secondary CH2 refined with riding coordinates:
 C5(H5D,H5E), C6(H6A,H6B), C7(H7A,H7B), C9B(H9BA,H9BB), C9A(H9AA,H9AB),
 C10A(H10A,H10B), C10B(H10C,H10D), C11A(H11B,H11C), C11B(H11A,H11D)
7.d Me refined with riding coordinates:
 N4(H4A,H4B,H4C)
;
_shelx_res_checksum              40128
_shelx_hkl_checksum              7028