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_7035838
_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         'C37 H45 Fe I P2 Si2'
_chemical_formula_sum            'C37 H45 Fe I P2 Si2'
_chemical_formula_weight         790.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8089(6)
_cell_length_b                   10.9073(3)
_cell_length_c                   28.9113(9)
_cell_measurement_reflns_used    11792
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.5377
_cell_measurement_theta_min      3.6169
_cell_volume                     7192.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega   -8.00   19.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127   38.0000  -60.0000 27

  2 omega   25.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000  -30.0000 90

  3 omega   42.00   85.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127 -108.0000   30.0000 43

  4 omega   38.00   74.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000    0.0000 36

  5 omega   86.00  149.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  150.0000 63

  6 omega   72.00  123.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -134.0000  135.0000 51

  7 omega   40.00   76.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   30.0000 36

  8 omega   83.00  109.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -108.0000 -149.0000 26

  9 omega   39.00   65.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   60.0000 26

 10 omega   38.00   77.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -60.0000 39

 11 omega   60.00  120.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000   90.0000 60

 12 omega   23.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000   60.0000 92

 13 omega  -27.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -38.0000 -120.0000 92

 14 omega   14.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   77.0000 -180.0000 101

 15 omega   66.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   15.0000   90.0000 25

 16 omega   83.00  116.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  -30.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0121286000
_diffrn_orient_matrix_UB_12      -0.0069797000
_diffrn_orient_matrix_UB_13      -0.0523686000
_diffrn_orient_matrix_UB_21      -0.0644158000
_diffrn_orient_matrix_UB_22      -0.0330562000
_diffrn_orient_matrix_UB_23      0.0099023000
_diffrn_orient_matrix_UB_31      -0.0161511000
_diffrn_orient_matrix_UB_32      0.1371795000
_diffrn_orient_matrix_UB_33      -0.0002604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.714
_diffrn_reflns_theta_min         3.620
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.763
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.2281
_exptl_crystal_size_mid          0.1036
_exptl_crystal_size_min          0.0151
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+6.1217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6078
_reflns_number_total             7197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           4I
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_database_code               7035838
_nottingham_internal_coll_name   FEACLU
_nottingham_internal_coll_number 10399
_nottingham_internal_coll_client AC/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '100.0000 and 25.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   1/6/2011
_nottingham_internal_process_date 02/06/2011
_nottingham_internal_process_user WL
_nottingham_internal_solution_date 02/06/2011
_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
_chemical_oxdiff_formula         'C37 H45 Fe P2 Si2 I'
_chemical_oxdiff_usercomment
'FEACLU #10399 IN FOMBLIN FILM ON MICROMOUNT FOR AC/STL'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.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), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              99883
_olex2_submission_special_instructions 'No special instructions were received'