Spontaneous dehydrocoupling in peri-substituted phosphine-borane adducts.
Taylor, Laurence J.; Surgenor, Brian A.; Wawrzyniak, Piotr; Ray, Matthew J.; Cordes, David B.; Slawin, Alexandra M. Z.; Kilian, Petr; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1976–1986; doi:10.1039/c5dt02539g

data_7036245
_publ_section_title
;
 Spontaneous dehydrocoupling in peri-substituted phosphine-borane adducts.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1976
_journal_page_last               1986
_journal_paper_doi               10.1039/c5dt02539g
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H36 B2 Fe P2'
_chemical_formula_sum            'C28 H36 B2 Fe P2'
_chemical_formula_weight         512.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-03
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2015-08-18 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.651(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.409(5)
_cell_length_b                   11.059(3)
_cell_length_c                   16.712(6)
_cell_measurement_reflns_used    4626
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.30
_cell_volume                     2588.3(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34241
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.569
_diffrn_reflns_theta_min         1.341
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.35
_refine_diff_density_min         -0.83
_refine_ls_abs_structure_details
;
 Flack x determined using 3167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, S., Flack, H. D and Wagner, T., Acta Cryst. B69 (2013) 249-259.).
;
_refine_ls_abs_structure_Flack   0.042(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0926P)^2^+29.0939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2572
_refine_ls_wR_factor_ref         0.2647
_reflns_number_gt                8212
_reflns_number_total             9417
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5dt02539g1.cif
_cod_data_source_block           5b
_cod_depositor_comments
'Adding full bibliography for 7036242--7036246.cif.'
_cod_database_code               7036245
_shelx_res_checksum              25399