Ferrocenyl-derived electrophilic phosphonium cations (EPCs) as Lewis acid catalysts.
Mallov, Ian; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5568–5574; doi:10.1039/c6dt00105j

data_7038427
_publ_section_title
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 Ferrocenyl-derived electrophilic phosphonium cations (EPCs) as Lewis acid
 catalysts.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5568
_journal_page_last               5574
_journal_paper_doi               10.1039/c6dt00105j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C34 H28 F2 Fe P2, 2(B C24 F20), C3.5 H3.5'
_chemical_formula_sum            'C85.5 H31.5 B2 F42 Fe P2'
_chemical_formula_weight         1996.08
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2015-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                74.451(2)
_cell_angle_beta                 87.233(2)
_cell_angle_gamma                89.862(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2251(8)
_cell_length_b                   16.3787(10)
_cell_length_c                   17.2783(11)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.42
_cell_volume                     3873.6(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.03
_diffrn_measured_fraction_theta_full 0.9930
_diffrn_measured_fraction_theta_max 0.9930
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67411
_diffrn_reflns_theta_full        27.5194
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0585 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.9705.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangualar
_exptl_crystal_F_000             1980.0156
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.1372
_refine_diff_density_min         -0.7100
_refine_diff_density_rms         0.1290
_refine_ls_d_res_high            0.7691
_refine_ls_d_res_low             11.0748
_refine_ls_goodness_of_fit_ref   1.0311
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         17730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0311
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+2.3230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                11616
_reflns_number_total             17730
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt00105j2.cif
_cod_data_source_block           IM034_0m
_cod_depositor_comments
'Adding full bibliography for 7038425--7038428.cif.'
_cod_database_code               7038427
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: H51(0.5) C54(0.5) H54(0.5) C50(0.5) H50(0.5) C53(0.5) H53(0.5)
 C56(0.5) C52(0.5) H52(0.5) C57(0.5) H57(0.5) C55(0.5) H55(0.5) C49(0.5)
 H49(0.5) C61(0.5) H61a(0.5) H61b(0.5) H61c(0.5)
 Fixed Uiso: H59(0.11938) H60(0.14453) H61a(0.10155) H61b(0.10155) H61c(0.10155)
3.a Ternary CH refined with riding coordinates:
 C27(H27), C28(H28), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C6aa(H6aa)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C3aa(H3aa), C0aa(H0aa), C2aa(H2aa), C4aa(H4aa),
 C5aa(H5aa), C51(H51), C54(H54), C50(H50), C53(H53), C52(H52), C57(H57),
 C55(H55), C49(H49), C59(H59), C60(H60)
3.c Idealised Me refined as rotating group:
 C61(H61a,H61b,H61c)
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_plat410_alert_2_a
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PROBLEM: Short Intra H...H Contact  H52    ..  H56   ...  1.31 Ang.
RESPONSE: No chemically meaningful explanation, results from disorder.
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_olex2_submission_special_instructions 'No special instructions were received'