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_7035835
_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         'C39 H45 Br Fe P2, 0.5(C7 H8)'
_chemical_formula_sum            'C42.5 H49 Br Fe P2'
_chemical_formula_weight         757.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 104.135(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0960(6)
_cell_length_b                   11.5845(4)
_cell_length_c                   21.4822(8)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.5101
_cell_measurement_theta_min      3.2356
_cell_volume                     3643.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -32.00   -2.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  125.0000   90.0000 30

  2 omega  -24.00   64.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -38.0000 -150.0000 88

  3 omega   23.00   99.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   57.0000    0.0000 76

  4 omega   23.00   58.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000 -109.0000 35

  5 omega   33.00   59.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   60.0000 26

  6 omega   49.00   75.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -60.0000 26

  7 omega   33.00   65.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  150.0000 32

  8 omega   34.00   68.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -30.0000 34

  9 omega   38.00   72.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   90.0000 34

 10 omega   44.00   99.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000   30.0000 55

 11 omega   33.00   68.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  120.0000 35

 12 omega   92.00  156.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   38.0000 -109.0000 64

 13 omega   38.00   64.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -90.0000 26

 14 omega  133.00  158.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000 -150.0000 25

 15 omega   35.00   68.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   30.0000 33

 16 omega  103.00  153.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  125.0000 -180.0000 50

 17 omega   90.00  145.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000    0.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0745059000
_diffrn_orient_matrix_UB_12      -0.0642562000
_diffrn_orient_matrix_UB_13      -0.0496925000
_diffrn_orient_matrix_UB_21      0.0643512000
_diffrn_orient_matrix_UB_22      -0.0072462000
_diffrn_orient_matrix_UB_23      -0.0456130000
_diffrn_orient_matrix_UB_31      0.0370591000
_diffrn_orient_matrix_UB_32      -0.1162314000
_diffrn_orient_matrix_UB_33      0.0303044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16175
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.683
_diffrn_reflns_theta_min         4.367
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.645
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.1566
_exptl_crystal_size_mid          0.0293
_exptl_crystal_size_min          0.0199
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7255
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+13.1285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             7255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           5Br
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_original_cell_volume        3643.0(2)
_cod_original_formula_sum        'C42.50 H49 Br Fe P2'
_cod_database_code               7035835
_nottingham_internal_coll_name   LHSSLF
_nottingham_internal_coll_number 11049
_nottingham_internal_coll_client AC/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   3/1/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date pczwl
_nottingham_internal_process_user 3/1/2012
_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         'C42.5 H49 Br Fe P2'
_chemical_oxdiff_usercomment
'LHSSLF #11049 IN FOMBLIN FILM ON MICROMOUNT FOR LHS/STL'
_reflns_odcompleteness_completeness 99.93
_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. Restrained distances
 C42-C40 \\sim C40-C46
 with sigma of 0.02
 C42-C41 \\sim C46-C41
 with sigma of 0.02
 C42-C43 \\sim C46-C45
 with sigma of 0.02
 C45-C44 \\sim C43-C44
 with sigma of 0.02
 C41-C43 \\sim C41-C45
 with sigma of 0.02
 C44-C46 \\sim C44-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C44 \\sim C45 \\sim C46 \\sim C41 \\sim C42 \\sim C43 \\sim C40: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C44(0.5) H44(0.5) C45(0.5) H45(0.5) C46(0.5) H46(0.5) C41(0.5)
 C42(0.5) H42(0.5) C43(0.5) H43(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
5.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),
 C44(H44), C45(H45), C46(H46), C42(H42), C43(H43)
5.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              64753
_olex2_submission_special_instructions 'No special instructions were received'