Rare Examples of Transition-Metal−Main-Group Metal Heterometallic Metal−Organic Frameworks from Gallium and Indium Dipyrrinato Complexes and Silver Salts: Synthesis and Framework Variability
Stork, Jay R.; Thoi, Van S.; Cohen, Seth M.; Inorganic Chemistry 46 (2007) 11213–11223; doi:10.1021/ic7016159

data_4333479
_publ_contact_author
;      Cohen, Seth M.
       Department of Chemistry and Biochemistry
       University of California, San Diego
       La Jolla
       CA 92093-0358
       USA
;
_publ_section_title
;
 Rare Examples of Transition-Metal&#x2212;Main-Group Metal Heterometallic
 Metal&#x2212;Organic Frameworks from Gallium and Indium Dipyrrinato
 Complexes and Silver Salts:&#x00A0; Synthesis and Framework Variability
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11213
_journal_page_last               11223
_journal_paper_doi               10.1021/ic7016159
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C42 H30 In N9, 1.5(C H Cl3)'
_chemical_formula_sum            'C43.5 H31 Cl4.5 In N9'
_chemical_formula_weight         954.12
_chemical_name_common            In(4-pyrdpm)~3~^.^1.5CHCl~3~
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.101(9)
_cell_angle_beta                 83.023(9)
_cell_angle_gamma                74.558(9)
_cell_formula_units_Z            2
_cell_length_a                   9.234(5)
_cell_length_b                   12.938(7)
_cell_length_c                   17.913(9)
_cell_measurement_reflns_used    1012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.66
_cell_volume                     2035.1(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       \w
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21925
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.96518
_exptl_absorpt_correction_T_min  0.77522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate-like needle'
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+2.4358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                7367
_reflns_number_total             8256
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic7016159sup1.cif
_cod_data_source_block           jrs131
_cod_original_cell_volume        2035.1(18)
_cod_original_formula_sum        'C43.50 H31 Cl4.50 In N9'
_cod_database_code               4333479