Halogen-bonded network of trinuclear copper(II) 4-iodopyrazolate complexes formed by mutual breakdown of chloroform and nanojars
Surmann, Stuart A.; Mezei, Gellert; Acta Crystallographica Section E 72 (2016) 1517–1520; doi:10.1107/S205698901601536X

data_2241868
_publ_section_title
;
 Halogen-bonded network of trinuclear copper(II) 4-iodopyrazolate
 complexes formed by mutual breakdown of chloroform and nanojars
;
_journal_coeditor_code           GK2666
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1517
_journal_page_last               1520
_journal_paper_doi               10.1107/S205698901601536X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'(C16 H36 N)2 [Cu3 Cl5 (C3 H2 I N2)3 Cl5], 0.5C4 H8 O'
_chemical_formula_moiety
'2(C16 H36 N +), C9 H6 Cl5 Cu3 I3 N6 2-, 0.5C4 H8 O'
_chemical_formula_sum            'C43 H82 Cl5 Cu3 I3 N8 O'
_chemical_formula_weight         1475.73
_chemical_name_systematic
;Bis(tetrabutylammonium)
di-\m~3~-chlorido-tris(\m-4-iodopyrazolato-\k^2^<i>N</i>:<i>N</i>')tris[chloridocuprate(II)] 1,4-dioxane hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                103.7070(10)
_cell_angle_beta                 90.4090(10)
_cell_angle_gamma                93.6540(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3604(2)
_cell_length_b                   11.5688(2)
_cell_length_c                   23.2200(3)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.21
_cell_volume                     2958.00(8)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2014)
;
_computing_publication_material
;
CrystalMaker (Palmer, 2014)
;
_computing_structure_refinement
;
<i>SHELXL2014/6</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            136857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         0.903
_exptl_absorpt_coefficient_mu    2.898
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.540
_refine_diff_density_min         -2.886
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         14685
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0646P)^2^+28.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                11845
_reflns_number_total             14685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gk2666sup1.cif
_cod_data_source_block           I
_cod_database_code               2241868
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.918
_shelx_hkl_checksum              91285
_shelx_res_checksum              9989
_shelxl_version_number           2014/6
_cod_database_fobs_code 2241868