Highly unusual interpenetration isomers of electroactive nickel bis(dithiolene) coordination frameworks
Thomas B. Faust; Pavel M. Usov; Deanna M. D'Alessandro; Cameron J. Kepert; Chem.Commun. 50 (2014) 12772–; doi:10.1039/C4cc05438E

data_7115786
_publ_section_title
;
 Highly unusual interpenetration isomers of electroactive nickel
 bis(dithiolene) coordination frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              12772
_journal_paper_doi               10.1039/C4cc05438E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 N4 Ni2 O2 S8 Zn'
_chemical_formula_sum            'C28 H20 N4 Ni2 O2 S8 Zn'
_chemical_formula_weight         883.75
_chemical_melting_point          ?
_chemical_name_common            '[Zn(Ni(pedt)2)2(O)2]'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   27.525(4)
_cell_length_b                   27.525(4)
_cell_length_c                   24.215(5)
_cell_measurement_temperature    100(2)
_cell_volume                     15888(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71085
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            230737
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.246
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_min         3.473
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker, 2012)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    0.554
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2676
_exptl_crystal_recrystallization_method 'Direct from synthesis'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.379
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 4698 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.117(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         21594
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      2.774
_refine_ls_R_factor_all          0.1734
_refine_ls_R_factor_gt           0.1182
_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^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2825
_refine_ls_wR_factor_ref         0.2922
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11612
_reflns_number_total             21594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05438e2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        15889(5)
_cod_database_code               7115786
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.982