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_7035826
_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         'C52 H48 Br4 Fe2 P4, 2(C7 H8)'
_chemical_formula_sum            'C66 H64 Br4 Fe2 P4'
_chemical_formula_weight         1412.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-16
_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            4
_cell_length_a                   18.7638(5)
_cell_length_b                   22.9601(5)
_cell_length_c                   14.2032(4)
_cell_measurement_reflns_used    8182
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.59
_cell_measurement_theta_min      3.66
_cell_volume                     6119.0(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   80.00  113.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   47.0000  132.0000 33

  2 omega  -24.00   50.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -57.0000  -30.0000 74

  3 omega  -21.00    5.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -38.0000  -30.0000 26

  4 omega   30.00   65.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -38.0000  -30.0000 35

  5 omega   75.00  110.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  -90.0000 35

  6 omega   48.00   77.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 29

  7 omega   38.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  120.0000 31

  8 omega   33.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -180.0000 36

  9 omega   33.00   68.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000    0.0000 35

 10 omega   43.00   93.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -120.0000 50

 11 omega  130.00  156.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472    0.0000   90.0000 26

 12 omega   31.00  107.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472    0.0000   90.0000 76
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0234087000
_diffrn_orient_matrix_UB_12      0.0204201000
_diffrn_orient_matrix_UB_13      -0.0986208000
_diffrn_orient_matrix_UB_21      -0.0705588000
_diffrn_orient_matrix_UB_22      -0.0336297000
_diffrn_orient_matrix_UB_23      0.0111024000
_diffrn_orient_matrix_UB_31      -0.0349026000
_diffrn_orient_matrix_UB_32      0.0543089000
_diffrn_orient_matrix_UB_33      0.0438234000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.151
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.213
_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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.2748
_exptl_crystal_size_mid          0.1491
_exptl_crystal_size_min          0.0552
_refine_diff_density_max         2.099
_refine_diff_density_min         -1.980
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5409
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.1321
_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^)+362.5271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3029
_refine_ls_wR_factor_ref         0.3037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5175
_reflns_number_total             5409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           IIa
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_database_code               7035826
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C66 H64 Br4 Fe2 P4'
_chemical_oxdiff_usercomment
'LHSSLE #11048 IN FOMBLIN FILM ON MICROMOUNT FOR LHS/STL'
_reflns_odcompleteness_completeness 99.88
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C26(H26A,H26B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_shelx_res_checksum              29545
_olex2_submission_special_instructions 'No special instructions were received'