Planar-chiral ferrocenylphosphine-borane complexes featuring agostic-type B‒H⋯E (E = Hg, Sn) interactions
Tagne Kuate, Alain C.; Lalancette, Roger A.; Jäkle, F.; Dalton Trans.  (2017) –; doi:10.1039/C6DT04791B

data_7042818
_publ_section_title
;
 Planar-chiral ferrocenylphosphine-borane complexes featuring agostic-type
 B--H&#x22EF;E (E = Hg, Sn) interactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04791B
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C46 H45 B Fe2 P2 Sn'
_chemical_formula_sum            'C46 H45 B Fe2 P2 Sn'
_chemical_formula_weight         900.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8780(2)
_cell_length_b                   17.5543(4)
_cell_length_c                   20.7334(5)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.293
_cell_measurement_theta_min      2.52
_cell_volume                     3959.16(15)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34745
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.819
_diffrn_reflns_theta_min         3.299
_exptl_absorpt_coefficient_mu    11.777
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2610 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                6561
_reflns_number_total             6872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04791b2.cif
_cod_data_source_block           AT64_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'dIfmap' changed to 'difmap'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7042818
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.130
_shelx_estimated_absorpt_t_max   0.241
_shelx_res_checksum              92828