Syntheses and Anion Binding Capabilities of Bis(diarylboryl) Ferrocenes and Related Systems
Kelly, Michael J.; Broomsgrove, Alexander E.J.; Morgan, Ian R.; Siewert, Inke; Fitzpatrick, Philip; Smart, Jessica; Vidovic, Dragoslav; Aldridge, Simon; Organometallics 32 (2013) 2674–; doi:10.1021/om400152x

data_4080751
_publ_section_title
;
 Syntheses and Anion Binding Capabilities of Bis(diarylboryl) Ferrocenes
 and Related Systems
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2674
_journal_paper_doi               10.1021/om400152x
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C47 H72.09 B1 Fe1 N2 O1 Si1'
_chemical_formula_sum            'C47 H72.09 B Fe N2 O Si'
_chemical_formula_weight         775.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90.3773(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.81313(12)
_cell_length_b                   17.36807(16)
_cell_length_c                   20.2116(2)
_cell_measurement_reflns_used    20141
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     4497.78(7)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48187
_diffrn_reflns_theta_full        75.036
_diffrn_reflns_theta_max         76.567
_diffrn_reflns_theta_min         3.355
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.196
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1684.348
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.54
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8767
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9346
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.0093968
_refine_ls_shift/su_mean         0.0002198
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.214E+04 0.352E+04 0.213E+04 862. 201. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1317
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1317
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8232
_reflns_number_total             9386
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.50
_oxford_diffrn_Wilson_scale      0.17
_oxford_refine_ls_r_factor_ref   0.0599
_oxford_refine_ls_scale          3.47(3)
_oxford_reflns_number_all        9347
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om400152x_si_002.cif
_cod_data_source_block           nBu4NfcBMes2CNSiMe2OH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.5 from 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4497.78(8)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C47 H72.09 B1 Fe1 N2 O1 Si1'
_cod_database_code               4080751
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   ( 302,X'S) H   (3021,X'S) H   (3022,X'S) 
RIDE C   ( 303,X'S) H   (3031,X'S) H   (3032,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE O   (  29,X'S) H   (  28,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) H   (2012,X'S) H   (2013,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   ( 200,X'S) H   (2001,X'S) H   (2002,X'S) H   (2003,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) H   (2112,X'S) H   (2113,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) H   (2102,X'S) H   (2103,X'S) 
RIDE C   ( 220,X'S) H   (2201,X'S) H   (2202,X'S) 
RIDE C   ( 221,X'S) H   (2211,X'S) H   (2212,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
REM CH3 
SAME C(2) SI(28) C(200) AND 
CONT C(2) SI(28) C(201) 
SIMU 0.01 C(2) SI(28) C(200) AND 
CONT C(2) SI(28) C(201) 
DELU 0.01 C(2) SI(28) C(200) AND 
CONT C(2) SI(28) C(201) 
REM TBA 
SAME C(302) C(220) C(210) AND 
CONT C(302) C(221) C(211) 
SIMU 0.01   C(302) C(220) C(210) AND 
CONT C(302) C(221) C(211) 
DELU 0.01   C(302) C(220) C(210) AND 
CONT C(302) C(221) C(211) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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