Synthesis and characterisation of halide, separated ion pair, and hydride cyclopentadienyl iron bis(diphenylphosphino)ethane derivatives.
Patel, Dipti; Wooles, Ashley; Cornish, Andrew D.; Steven, Lindsey; Davies, E. Stephen; Evans, David J.; McMaster, Jonathan; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14159–14177; doi:10.1039/c5dt00704f

data_7035837
_publ_section_title
;
 Synthesis and characterisation of halide, separated ion pair, and hydride
 cyclopentadienyl iron bis(diphenylphosphino)ethane derivatives.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14159
_journal_page_last               14177
_journal_paper_doi               10.1039/c5dt00704f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C34 H37 Fe I P2 Si, 0.5(C7 H8)'
_chemical_formula_sum            'C37.5 H41 Fe I P2 Si'
_chemical_formula_weight         764.48
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-11 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                106.3660(10)
_cell_angle_beta                 103.3670(10)
_cell_angle_gamma                104.0210(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5992(9)
_cell_length_b                   12.5015(11)
_cell_length_c                   14.6903(13)
_cell_measurement_reflns_used    6306
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.501
_cell_measurement_theta_min      2.265
_cell_volume                     1715.7(3)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15274
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0566 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.8910.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7740
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0347P)^2^+1.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6863
_reflns_number_total             7740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           3I
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_original_formula_sum        'C37.50 H41 Fe I P2 Si'
_cod_database_code               7035837
_nottingham_internal_coll_name   FEACMD
_nottingham_internal_coll_number 10736
_nottingham_internal_coll_client AC/STL
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_frame_time 30
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_user   AC
_nottingham_internal_coll_date   26/9/2011
_nottingham_internal_process_date 17/11/2011
_nottingham_internal_process_user WL
_nottingham_internal_solution_date 17/11/2011
_nottingham_internal_solution_user AC
_nottingham_internal_refinement_date 6/5/2015
_nottingham_internal_refinement_user pczwl
_nottingham_internal_validation_date 6/5/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 6/5/2015
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C35 \\sim C35-C41
 with sigma of 0.02
 C38-C36 \\sim C36-C40
 with sigma of 0.02
 C37-C39 \\sim C39-C41
 with sigma of 0.02
 C37-C36 \\sim C41-C36
 with sigma of 0.02
 C38-C37 \\sim C41-C40
 with sigma of 0.02
 C39-C38 \\sim C40-C39
 with sigma of 0.02
3. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C36(0.5) C37(0.5) H37(0.5)
 C38(0.5) H38(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34C,H34A,H34B), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              20693
_olex2_submission_special_instructions 'No special instructions were received'