Crystal structure of <i>catena</i>-poly[bis(tetraethylammonium) [tetraaquatris(μ-dicyanamido-κ^2^<i>N</i>^1^:<i>N</i>^5^)bis(dicyanamido-κ<i>N</i>^1^)dicobaltate(II)] dicyanamide]
Liu, Chen; Thuijs, Annaliese E.; Abboud, Khalil A.; Acta Crystallographica Section E 72 (2016) 1603–1606; doi:10.1107/S2056989016016637

data_2241894
_publ_section_title
;
 Crystal structure of <i>catena</i>-poly[bis(tetraethylammonium)
 [tetraaquatris(\m-dicyanamido-\k^2^<i>N</i>^1^:<i>N</i>^5^)bis(dicyanamido-\k<i>N</i>^1^)dicobaltate(II)]
 dicyanamide]
;
_journal_coeditor_code           WM5330
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1603
_journal_page_last               1606
_journal_paper_doi               10.1107/S2056989016016637
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '(C8 H20 N)2 [Co2 (C2 N3)5 (H2 O1)4] (C2 N3)'
_chemical_formula_moiety         '2(C8 H20 N1 +), C10 H8 Co2 N15 O4, C2 N3 -'
_chemical_formula_sum            'C28 H48 Co2 N20 O4'
_chemical_formula_weight         846.72
_chemical_name_systematic
;<i>catena</i>-Poly[bis(tetraethylammonium)
[tetraaquatris(\m-dicyanamido-\k^2^<i>N</i>^1^:<i>N</i>^5^)bis(dicyanamido-\k<i>N</i>^1^)dicobaltate(II)] dicyanamide]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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
_cell_angle_beta                 94.4257(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9836(19)
_cell_length_b                   7.3271(6)
_cell_length_c                   22.6809(17)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3973.8(5)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL-plus (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII DUO CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26031
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         1.703
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.9469
_exptl_absorpt_correction_T_min  0.8980
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
based on measured indexed crystal faces
(SHELXTL2014; Sheldrick, 2015<i>a</i>)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.216
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3859 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         9018
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0456P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                8397
_reflns_number_total             9018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5330sup1.cif
_cod_data_source_block           I
_cod_database_code               2241894
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              55054
_shelx_res_checksum              44653
_cod_database_fobs_code 2241894