Evaluation of Electronics, Electrostatics and Hydrogen Bond Cooperativity in the Binding of Cyanide and Fluoride by Lewis Acidic Ferrocenylboranes
Alexander E. J. Broomsgrove; David A. Addy; Angela Di Paolo; Ian R. Morgan; Christopher Bresner; Victoria Chislett; Ian A. Fallis; Amber L. Thompson; Dragoslav Vidovic; Simon Aldridge; Inorganic Chemistry 49 (2010) 157–173; doi:10.1021/ic901673u

data_4314455
_publ_contact_author             'Simon Aldridge'
_publ_section_title
;
 Evaluation of Electronics, Electrostatics and Hydrogen Bond Cooperativity
 in the Binding of Cyanide and Fluoride by Lewis Acidic Ferrocenylboranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              157
_journal_page_last               173
_journal_paper_doi               10.1021/ic901673u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C41 H54.96 B1 Br0.04 Fe1 K1 N1 O8'
_chemical_formula_sum            'C41 H54.96 B Br0.04 Fe K N O8'
_chemical_formula_weight         798.76
_chemical_melting_point          ?
_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
_audit_creation_date             09-08-15
_audit_creation_method           CRYSTALS_ver_12.90
_cell_angle_alpha                90
_cell_angle_beta                 97.5901(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0544(1)
_cell_length_b                   27.3288(3)
_cell_length_c                   12.4741(2)
_cell_measurement_reflns_used    8837
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4073.37(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46021
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1693.361
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9208
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.0007395
_refine_ls_shift/su_mean         0.0001329
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 4.93P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1315
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1315
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                7167
_reflns_number_total             9208
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.71
_oxford_diffrn_Wilson_scale      10.00
_oxford_refine_ls_r_factor_ref   0.0831
_oxford_refine_ls_scale          0.3132(3)
_oxford_reflns_number_all        9208
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 096abdv09
_cod_data_source_file            ic901673u_si_002_12.cif
_cod_data_source_block           '[K(18-crown-6)]+[5.CN]-'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z 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 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C41 H54.96 B1 Br0.04 Fe1 K1 N1 O8'
_cod_database_code               4314455