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_4312620
_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            'C29 H28 Fe I N2 O P Zn'
_chemical_formula_weight         699.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.362(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.936(4)
_cell_length_b                   15.982(6)
_cell_length_c                   16.338(6)
_cell_measurement_temperature    110(2)
_cell_volume                     2855.5(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1461
_diffrn_reflns_av_sigmaI/netI    0.1958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14607
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_refine_diff_density_max         8.520
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.641
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5017
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.604
_refine_ls_R_factor_all          0.2795
_refine_ls_R_factor_gt           0.2084
_refine_ls_shift/su_max          0.439
_refine_ls_shift/su_mean         0.057
_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          0.5187
_refine_ls_wR_factor_ref         0.5354
_reflns_number_gt                2374
_reflns_number_total             5017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347900_s1_1.cif
_cod_data_source_block           ja1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        2855.3(19)
_cod_database_code               4312620