Synthesis and Structural Characterization of Double Metal Cyanides of Iron and Zinc: Catalyst Precursors for the Copolymerization of Carbon Dioxide and Epoxides
Donald J. Darensbourg; M. Jason Adams; Jason C. Yarbrough; Andrea L. Phelps; Inorganic Chemistry 42 (2003) 7809–7818; doi:10.1021/ic0347900

data_4312621
_publ_section_title
;
 Synthesis and Structural Characterization of Double Metal Cyanides of
 Iron and Zinc: Catalyst Precursors for the Copolymerization of Carbon
 Dioxide and Epoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7809
_journal_page_last               7818
_journal_paper_doi               10.1021/ic0347900
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C125 H105 Ag2 Fe4 I4 N13 P4 Zn3'
_chemical_formula_weight         2821.30
_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                63.302(6)
_cell_angle_beta                 69.002(6)
_cell_angle_gamma                79.220(6)
_cell_formula_units_Z            2
_cell_length_a                   14.240(4)
_cell_length_b                   16.089(5)
_cell_length_c                   17.644(5)
_cell_measurement_temperature    110(2)
_cell_volume                     3369.9(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.2368
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13358
_diffrn_reflns_theta_full        23.23
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.835
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1517
_refine_diff_density_max         3.615
_refine_diff_density_min         -2.192
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         9409
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      2.178
_refine_ls_R_factor_all          0.2637
_refine_ls_R_factor_gt           0.1902
_refine_ls_shift/su_max          15.000
_refine_ls_shift/su_mean         0.215
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4874
_refine_ls_wR_factor_ref         0.5102
_reflns_number_gt                4351
_reflns_number_total             9409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347900_s1_2.cif
_cod_data_source_block           ja1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3370.1(17)
_cod_database_code               4312621