Three Guest-Including Coordination Solids from a Single Crystallization: A Discrete Cage and Open-Channel Networks from 1-D Ladders and 1-D Ribbons
Amir H. Mahmoudkhani; George K. H. Shimizu; Inorganic Chemistry 46 (2007) 1593–1602; doi:10.1021/ic0615123

data_4307009
_publ_contact_author_address
; 
Department of Chemistry, University of Calgary, Calgary, AB, Canada
;
_publ_contact_author_email       gshimizu@ucalgary.ca
_publ_contact_author_fax         +1-403-3912350
_publ_contact_author_name        'George K. H. Shimizu'
_publ_contact_author_phone       +1-403-2205344
_publ_section_title
;
Three Guest-Including Coordination Solids from a Single Crystallization:
A Discrete Cage and Open-Channel Networks from 1-D Ladders and 1-D Ribbons
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1593
_journal_page_last               1602
_journal_paper_doi               10.1021/ic0615123
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C115 H99 Cu3 N13.4 O19 S6'
_chemical_formula_weight         2355.66
_chemical_name_systematic
;
 ?
;
_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                108.91(3)
_cell_angle_beta                 93.16(3)
_cell_angle_gamma                90.43(3)
_cell_formula_units_Z            1
_cell_length_a                   10.510(2)
_cell_length_b                   14.158(3)
_cell_length_c                   21.748(4)
_cell_measurement_reflns_used    22373
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      1
_cell_volume                     3055.7(12)
_computing_cell_refinement       'HKL Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1998)'
_computing_data_reduction        'Scalepack (Otwinowski & Minor,1997)'
_computing_molecular_graphics    'Diamond 2.1d (Brandenbrg, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\w and \f 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  0.049
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18692
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         9667
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.111
_refine_ls_R_factor_gt           0.079
_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^)+(0.1526P)^2^+3.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.223
_refine_ls_wR_factor_ref         0.249
_reflns_number_gt                6864
_reflns_number_total             9667
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0615123si20060814_082822_2.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        3055.8(11)
_cod_original_formula_sum        'C115 H99 Cu3 N13.40 O19 S6'
_cod_database_code               4307009