Trinuclear Copper(I) and Silver(I) Adducts of 4-Chloro-3,5-bis(trifluoromethyl)pyrazolate and 4-Bromo-3,5-bis(trifluoromethyl)pyrazolate
Champika V. Hettiarachchi; Manal A. Rawashdeh-Omary; Daniel Korir; Jehan Kohistani; Muhammed Yousufuddin; H. V. Rasika Dias; Inorganic Chemistry 52 (2013) 13576–13583; doi:10.1021/ic402080y

data_4336871
_publ_contact_author_address
;Department of Chemistry and Biochemistry
The University of Texas at Arlington
700 Planetarium Place, Room 130 CPB
Arlington, Texas 76019-0065, USA
;
_publ_contact_author_email       dias@uta.edu
_publ_contact_author_fax         817-272-3808
_publ_contact_author_name        'Rasika Dias'
_publ_contact_author_phone       817-272-3813
_publ_section_title
;
 Trinuclear Copper(I) and Silver(I) Adducts of
 4-Chloro-3,5-bis(trifluoromethyl)pyrazolate and
 4-Bromo-3,5-bis(trifluoromethyl)pyrazolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13576
_journal_page_last               13583
_journal_paper_doi               10.1021/ic402080y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C15 Br3 Cu3 F18 N6'
_chemical_formula_sum            'C15 Br3 Cu3 F18 N6'
_chemical_formula_weight         1036.56
_chemical_name_common            {[4-Br-3,5-(CF3)2Pz]Cu}3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.557(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.054(4)
_cell_length_b                   23.633(7)
_cell_length_c                   16.525(5)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.654
_cell_measurement_theta_min      2.314
_cell_volume                     5357(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55755
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.567
_diffrn_reflns_theta_min         1.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.983
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1564 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.5920.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear whitish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_density_diffrn    2.570
_exptl_crystal_description       plate
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         14587
_refine_ls_number_restraints     798
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0502P)^2^+1.7284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7202
_reflns_number_total             14587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402080y_si_002_3.cif
_cod_data_source_block           dias878s
_cod_database_code               4336871
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.336
_shelx_hkl_checksum              20274