Inclusion of a dithiadiazolyl radical in a seemingly non-porous solid
Nikolayenko, Varvara I.; Barbour, Leonard J.; Arauzo, Ana; Campo, Javier; Rawson, Jeremy M.; Haynes, Delia A.; Chem. Commun.  (2017) –; doi:10.1039/C7CC06678C

data_7120722
_publ_section_title
;
 Inclusion of a dithiadiazolyl radical in a seemingly non-porous solid
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06678C
_journal_year                    2017
_chemical_formula_moiety         'C34 H40 Cl4 Cu2 N8, 0.606(C7 H5 N2 S2)'
_chemical_formula_sum            'C38.24 H43.03 Cl4 Cu2 N9.21 S1.21'
_chemical_formula_weight         939.34
_chemical_name_common            CuBx_PhCNSSN_100K
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-08-04 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.147(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.361(3)
_cell_length_b                   10.911(4)
_cell_length_c                   22.138(8)
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5325
_cell_measurement_theta_min      2.4675
_cell_volume                     1993.9(13)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX CCD area -detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11435
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.213
_diffrn_reflns_theta_min         1.863
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.9275
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, 2016'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       Block
_exptl_crystal_F_000             964.7
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0429P)^2^+1.0132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3225
_reflns_number_total             4600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06678c2.cif
_cod_data_source_block           CuBx_PhCNSSN_100K
_cod_database_code               7120722
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.653
_shelx_estimated_absorpt_t_max   0.851
_shelx_res_checksum              75108