Clathrochelate monoribbed-functionalized iron(ii) α-dioximates: synthetic pathways and structural and electrochemical features
Voloshin, Yan Z.; Zavodnik, Valery E.; Varzatskii, Oleg A.; Belsky, Vitaly K.; Palchik, Aleksei V.; Strizhakova, Nataly G.; Vorontsov, Ivan I.; Antipin, Mikhail Yu.; Journal of the Chemical Society, Dalton Transactions  (2002) 1193–; doi:10.1039/b107021p

data_7702698
_publ_section_title
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 Clathrochelate monoribbed-functionalized iron(ii) \a-dioximates:
 synthetic pathways and structural and electrochemical features
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1193
_journal_paper_doi               10.1039/b107021p
_journal_year                    2002
_chemical_formula_sum            'C40 H36 B2 Cl F2 Fe N7 O6'
_chemical_formula_weight         861.68
_chemical_name_systematic
;
1,8-Bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza-
4,5,11,12-tetraphenyl-17-chloro-18-diethylaminobicyclo-[6.6.6]eicosa-
3,5,10,12,16,18-hexaene iron(II)x(C6H6)
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           Orthorombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.077(3)
_cell_length_b                   21.551(4)
_cell_length_c                   21.580(4)
_cell_measurement_reflns_used    118
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     7942(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL PLUS 5.0'
_computing_publication_material  'SHELXTL PLUS 5.0'
_computing_structure_refinement  'SHELXTL PLUS 5.0'
_computing_structure_solution    'SHELXTL PLUS 5.0'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Bruker SMART 1K CCC'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54556
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.779164
_exptl_absorpt_correction_type   'semi-empirical (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.206
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_obs          0.0635
_refine_ls_shift/esd_max         0.129
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+2.3045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2201
_refine_ls_wR_factor_obs         0.1884
_reflns_number_observed          5883
_reflns_number_total             9138
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107021p.txt
_cod_data_source_block           9
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+2.3045P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+2.3045P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        7942.1(24)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7702698