M(μ-CN)Fe(μ-CN)M' Chains with Phthalocyanine Iron Centers: Preparation, Structures, and Isomerization
Andreas Geiss; Heinrich Vahrenkamp; Inorganic Chemistry 39 (2000) 4029–4036; doi:10.1021/ic0001412

data_4321303
_publ_section_title
;
 M(\m-CN)Fe(\m-CN)M' Chains with Phthalocyanine Iron Centers: Preparation,
 Structures, and Isomerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4029
_journal_page_last               4036
_journal_paper_doi               10.1021/ic0001412
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C96 H74 F6 Fe3 N10 P4 Sb'
_chemical_formula_weight         1894.83
_chemical_name_common            '[{FeCp(dppe)-CN}2-FePc]SbF6'
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.935(4)
_cell_length_b                   9.0170(10)
_cell_length_c                   25.538(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4322.7(16)
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  NONIUS-TURBO-CAD4
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.1057
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8662
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.40
_diffrn_standards_interval_count 'OCR every 200 refl.'
_diffrn_standards_interval_time  'ICR every 7200s'
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1926
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+4.8447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                4486
_reflns_number_total             8465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0001412_4.cif
_cod_data_source_block           g10(c9a)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (84 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (165
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+4.8447P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+4.8447P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321303