Halide and Nitrite Recognizing Hexanuclear Metallacycle Copper(II) Pyrazolates
Ahmed A. Mohamed; Simone Ricci; Alfredo Burini; Rossana Galassi; Carlo Santini; Gina M. Chiarella; Doris Y. Melgarejo; John P. Fackler; Inorganic Chemistry 50 (2011) 1014–1020; doi:10.1021/ic1016824

data_4324337
_publ_section_title
;
 Halide and Nitrite Recognizing Hexanuclear Metallacycle Copper(II)
 Pyrazolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1014
_journal_page_last               1020
_journal_paper_doi               10.1021/ic1016824
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C30 H12 Cu6 F36 I N12 O6, C16 H36 N, C6 H11, C6 H14'
_chemical_formula_sum            'C58 H73 Cu6 F36 I N13 O6'
_chemical_formula_weight         2240.49
_chemical_name_systematic
; 

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;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.777(2)
_cell_angle_beta                 98.994(2)
_cell_angle_gamma                91.077(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5997(16)
_cell_length_b                   12.7588(16)
_cell_length_c                   25.747(3)
_cell_measurement_reflns_used    8846
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.26
_cell_volume                     4077.5(9)
_computing_cell_refinement       'APEX-II (BRUKER-NONIUS, 2008)'
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2008)'
_computing_data_reduction        'APEX-II (BRUKER-NONIUS, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'SHELXTL (Bruker 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37876
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       block
_exptl_crystal_F_000             2222
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.248
_refine_diff_density_min         -2.358
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         13736
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.807
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+6.4103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                10422
_reflns_number_total             13736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016824_si_001_3.cif
_cod_data_source_block           crown_I
_cod_original_cell_volume        4077.4(9)
_cod_original_formula_sum        'C58 H73 Cu6 F36 I N13 O6 '
_cod_database_code               4324337