#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312620.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312620
loop_
_publ_author_name
'Donald J. Darensbourg'
'M. Jason Adams'
'Jason C. Yarbrough'
'Andrea L. Phelps'
_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/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.8004(5) 0.9336(2) 0.3510(2) 0.0652(15) Uani 1 1 d . . .
I1 I 0.7421(3) 0.97728(14) 0.20938(11) 0.0599(10) Uani 1.038(10) 1 d P A 1
O1 O 0.751(2) 0.8099(17) 0.3630(14) 0.088(3) Uani 1.038(10) 1 d PDU A 1
C1D C 0.6891(8) 0.7693(18) 0.4228(11) 0.090(3) Uani 1.038(10) 1 d PDU A 1
H1DA H 0.6038 0.7594 0.4047 0.108 Uiso 1.038(10) 1 calc PR A 1
H1DB H 0.6870 0.8047 0.4726 0.108 Uiso 1.038(10) 1 calc PR A 1
C2D C 0.846(3) 0.684(2) 0.401(2) 0.092(3) Uani 1.038(10) 1 d PDU A 1
H2DA H 0.8649 0.6275 0.3805 0.110 Uiso 1.038(10) 1 calc PR A 1
H2DB H 0.9173 0.7051 0.4332 0.110 Uiso 1.038(10) 1 calc PR A 1
C3D C 0.751(4) 0.684(2) 0.444(2) 0.091(3) Uani 1.038(10) 1 d PDU A 1
H3DA H 0.7708 0.6805 0.5027 0.109 Uiso 1.038(10) 1 calc PR A 1
H3DB H 0.6969 0.6369 0.4284 0.109 Uiso 1.038(10) 1 calc PR A 1
C4D C 0.814(3) 0.745(2) 0.3296(16) 0.091(3) Uani 1.038(10) 1 d PDU A 1
H4DA H 0.8897 0.7658 0.3033 0.109 Uiso 1.038(10) 1 calc PR A 1
H4DB H 0.7637 0.7162 0.2878 0.109 Uiso 1.038(10) 1 calc PR A 1
Fe1 Fe 0.7476(4) 1.0469(2) 0.6237(2) 0.0339(12) Uani 1 1 d . . .
N1 N 0.733(2) 0.9811(14) 0.4505(12) 0.036(4) Uani 1 1 d U A .
N2 N 0.988(4) 0.926(2) 0.3713(16) 0.083(6) Uani 1 1 d U A .
P1 P 0.7571(8) 0.9202(5) 0.6733(4) 0.039(2) Uani 1 1 d . . .
C1 C 0.743(3) 1.0045(17) 0.5189(15) 0.036(4) Uani 1 1 d U . .
C2 C 1.101(5) 0.938(3) 0.373(2) 0.082(6) Uani 1 1 d U . .
C1A C 0.705(2) 1.1129(15) 0.7303(13) 0.073(3) Uani 1 1 d DU . .
H1AA H 0.7441 1.1055 0.7852 0.087 Uiso 1 1 calc R A .
C2A C 0.746(2) 1.1691(15) 0.6657(13) 0.072(3) Uani 1 1 d DU A .
H2AA H 0.8176 1.2076 0.6688 0.086 Uiso 1 1 calc R . .
C3A C 0.663(2) 1.1599(16) 0.5959(14) 0.072(3) Uani 1 1 d DU . .
H3AA H 0.6679 1.1907 0.5427 0.087 Uiso 1 1 calc R A .
C4A C 0.572(2) 1.0961(17) 0.6168(15) 0.073(3) Uani 1 1 d DU A .
H4AA H 0.5042 1.0757 0.5805 0.088 Uiso 1 1 calc R . .
C5A C 0.593(2) 1.0716(17) 0.7017(15) 0.073(3) Uani 1 1 d DU A .
H5AA H 0.5455 1.0287 0.7326 0.088 Uiso 1 1 calc R . .
C1C C 0.904(3) 0.855(2) 0.649(2) 0.066(3) Uani 1 1 d DU . .
C2C C 0.940(3) 0.8007(19) 0.702(2) 0.067(3) Uani 1 1 d DU . .
H2CA H 0.9000 0.7973 0.7537 0.081 Uiso 1 1 calc R . .
C3C C 1.044(3) 0.743(2) 0.682(2) 0.068(3) Uani 1 1 d DU . .
H3CA H 1.0748 0.7031 0.7208 0.082 Uiso 1 1 calc R . .
C4C C 1.090(3) 0.751(2) 0.607(2) 0.068(3) Uani 1 1 d DU . .
H4CA H 1.1496 0.7122 0.5890 0.081 Uiso 1 1 calc R . .
C5C C 1.049(3) 0.817(2) 0.554(2) 0.067(3) Uani 1 1 d DU . .
H5CA H 1.0916 0.8260 0.5045 0.081 Uiso 1 1 calc R . .
C6C C 0.952(3) 0.867(2) 0.571(2) 0.067(3) Uani 1 1 d DU . .
H6CA H 0.9206 0.9069 0.5336 0.080 Uiso 1 1 calc R . .
C7C C 0.7791(17) 0.9224(17) 0.7825(11) 0.069(3) Uani 1 1 d DU . .
C8C C 0.8877(18) 0.9464(16) 0.8191(11) 0.070(3) Uani 1 1 d DU . .
H8CA H 0.9560 0.9601 0.7861 0.084 Uiso 1 1 calc R . .
C9C C 0.8979(19) 0.9506(18) 0.9040(12) 0.072(3) Uani 1 1 d DU . .
H9CA H 0.9742 0.9632 0.9291 0.086 Uiso 1 1 calc R . .
C10C C 0.795(2) 0.936(2) 0.9512(12) 0.071(3) Uani 1 1 d DU . .
H10A H 0.7963 0.9497 1.0078 0.086 Uiso 1 1 calc R . .
C11C C 0.691(2) 0.902(2) 0.9154(12) 0.072(3) Uani 1 1 d DU . .
H11A H 0.6296 0.8769 0.9484 0.087 Uiso 1 1 calc R . .
C12C C 0.677(2) 0.905(2) 0.8308(12) 0.070(3) Uani 1 1 d DU . .
H12A H 0.5997 0.8945 0.8061 0.084 Uiso 1 1 calc R . .
C13C C 0.642(4) 0.851(2) 0.6521(18) 0.072(3) Uani 1 1 d DU . .
C14C C 0.652(4) 0.758(2) 0.6557(16) 0.073(3) Uani 1 1 d DU . .
H14A H 0.7299 0.7351 0.6694 0.087 Uiso 1 1 calc R . .
C15C C 0.562(4) 0.704(2) 0.6412(18) 0.074(3) Uani 1 1 d DU . .
H15A H 0.5746 0.6453 0.6424 0.089 Uiso 1 1 calc R . .
C16C C 0.444(4) 0.739(2) 0.624(2) 0.074(3) Uani 1 1 d DU . .
H16A H 0.3751 0.7026 0.6192 0.089 Uiso 1 1 calc R . .
C17C C 0.427(4) 0.823(2) 0.614(2) 0.074(3) Uani 1 1 d DU . .
H17A H 0.3512 0.8460 0.5951 0.089 Uiso 1 1 calc R . .
C18C C 0.526(4) 0.872(2) 0.632(2) 0.073(3) Uani 1 1 d DU . .
H18A H 0.5107 0.9309 0.6312 0.088 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 O1 101.2(9) . . ?
N1 Zn1 N2 105.5(11) . . ?
O1 Zn1 N2 101.0(12) . . ?
N1 Zn1 I1 124.8(7) . . ?
O1 Zn1 I1 106.9(7) . . ?
N2 Zn1 I1 114.2(8) . . ?
C1D O1 C4D 101(2) . . ?
C1D O1 Zn1 131.3(18) . . ?
C4D O1 Zn1 124(2) . . ?
O1 C1D C3D 111.0(15) . . ?
C3D C2D C4D 103.2(16) . . ?
C2D C3D C1D 103.9(15) . . ?
O1 C4D C2D 106.6(18) . . ?
C2 Fe1 C1 96.0(15) 3_776 . ?
C2 Fe1 C4A 149.3(16) 3_776 . ?
C1 Fe1 C4A 94.0(12) . . ?
C2 Fe1 C2A 82.2(15) 3_776 . ?
C1 Fe1 C2A 130.9(10) . . ?
C4A Fe1 C2A 69.5(9) . . ?
C2 Fe1 C3A 108.7(16) 3_776 . ?
C1 Fe1 C3A 96.2(10) . . ?
C4A Fe1 C3A 41.2(6) . . ?
C2A Fe1 C3A 41.2(6) . . ?
C2 Fe1 C1A 97.3(13) 3_776 . ?
C1 Fe1 C1A 162.7(12) . . ?
C4A Fe1 C1A 69.0(9) . . ?
C2A Fe1 C1A 41.1(6) . . ?
C3A Fe1 C1A 69.0(8) . . ?
C2 Fe1 C5A 137.0(13) 3_776 . ?
C1 Fe1 C5A 126.9(13) . . ?
C4A Fe1 C5A 40.2(6) . . ?
C2A Fe1 C5A 67.8(9) . . ?
C3A Fe1 C5A 67.7(9) . . ?
C1A Fe1 C5A 40.1(6) . . ?
C2 Fe1 P1 94.5(15) 3_776 . ?
C1 Fe1 P1 90.3(8) . . ?
C4A Fe1 P1 114.4(8) . . ?
C2A Fe1 P1 138.8(7) . . ?
C3A Fe1 P1 155.0(8) . . ?
C1A Fe1 P1 99.7(7) . . ?
C5A Fe1 P1 89.2(8) . . ?
C1 N1 Zn1 152(2) . . ?
C2 N2 Zn1 166(3) . . ?
C13C P1 C7C 107.9(13) . . ?
C13C P1 C1C 102.6(17) . . ?
C7C P1 C1C 96.2(13) . . ?
C13C P1 Fe1 119.5(14) . . ?
C7C P1 Fe1 110.8(9) . . ?
C1C P1 Fe1 117.0(11) . . ?
N1 C1 Fe1 175(3) . . ?
N2 C2 Fe1 179(3) . 3_776 ?
C2A C1A C5A 107.9(7) . . ?
C2A C1A Fe1 68.7(10) . . ?
C5A C1A Fe1 72.4(12) . . ?
C1A C2A C3A 108.1(7) . . ?
C1A C2A Fe1 70.3(10) . . ?
C3A C2A Fe1 69.8(10) . . ?
C4A C3A C2A 107.9(7) . . ?
C4A C3A Fe1 69.4(12) . . ?
C2A C3A Fe1 69.0(10) . . ?
C5A C4A C3A 107.7(7) . . ?
C5A C4A Fe1 72.8(14) . . ?
C3A C4A Fe1 69.4(12) . . ?
C1A C5A C4A 108.1(8) . . ?
C1A C5A Fe1 67.4(11) . . ?
C4A C5A Fe1 67.0(13) . . ?
C2C C1C C6C 127(3) . . ?
C2C C1C P1 117(3) . . ?
C6C C1C P1 115(3) . . ?
C1C C2C C3C 120(3) . . ?
C4C C3C C2C 115(3) . . ?
C3C C4C C5C 121(3) . . ?
C6C C5C C4C 123(3) . . ?
C5C C6C C1C 114(3) . . ?
C8C C7C C12C 119.9(10) . . ?
C8C C7C P1 123.0(12) . . ?
C12C C7C P1 117.0(12) . . ?
C7C C8C C9C 120.6(10) . . ?
C10C C9C C8C 119.1(10) . . ?
C9C C10C C11C 119.8(10) . . ?
C12C C11C C10C 119.2(11) . . ?
C11C C12C C7C 119.1(10) . . ?
C18C C13C C14C 109(4) . . ?
C18C C13C P1 125(3) . . ?
C14C C13C P1 126(3) . . ?
C15C C14C C13C 126(4) . . ?
C14C C15C C16C 117(4) . . ?
C15C C16C C17C 122(4) . . ?
C18C C17C C16C 115(4) . . ?
C13C C18C C17C 130(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 1.94(2) . ?
Zn1 O1 2.06(3) . ?
Zn1 N2 2.08(4) . ?
Zn1 I1 2.496(5) . ?
O1 C1D 1.36(2) . ?
O1 C4D 1.36(3) . ?
C1D C3D 1.55(4) . ?
C2D C3D 1.26(5) . ?
C2D C4D 1.56(4) . ?
Fe1 C2 1.67(5) 3_776 ?
Fe1 C1 1.84(3) . ?
Fe1 C4A 2.08(3) . ?
Fe1 C2A 2.07(2) . ?
Fe1 C3A 2.08(3) . ?
Fe1 C1A 2.09(2) . ?
Fe1 C5A 2.16(3) . ?
Fe1 P1 2.183(8) . ?
N1 C1 1.18(3) . ?
N2 C2 1.25(6) . ?
P1 C13C 1.71(4) . ?
P1 C7C 1.80(2) . ?
P1 C1C 1.96(3) . ?
C2 Fe1 1.67(5) 3_776 ?
C1A C2A 1.46(2) . ?
C1A C5A 1.46(2) . ?
C2A C3A 1.46(2) . ?
C3A C4A 1.46(2) . ?
C4A C5A 1.46(2) . ?
C1C C2C 1.29(5) . ?
C1C C6C 1.39(5) . ?
C2C C3C 1.51(5) . ?
C3C C4C 1.33(5) . ?
C4C C5C 1.44(5) . ?
C5C C6C 1.35(5) . ?
C7C C8C 1.380(16) . ?
C7C C12C 1.399(17) . ?
C8C C9C 1.392(16) . ?
C9C C10C 1.385(17) . ?
C10C C11C 1.393(17) . ?
C11C C12C 1.391(17) . ?
C13C C18C 1.35(5) . ?
C13C C14C 1.49(5) . ?
C14C C15C 1.33(5) . ?
C15C C16C 1.43(5) . ?
C16C C17C 1.37(5) . ?
C17C C18C 1.38(5) . ?
