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_7035839
_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 Fe I P2, 0.5(C7 H8)'
_chemical_formula_sum            'C42.5 H49 Fe I P2'
_chemical_formula_weight         804.50
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-06
_audit_creation_method
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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                 104.489(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3141(9)
_cell_length_b                   11.6027(7)
_cell_length_c                   21.5557(15)
_cell_measurement_reflns_used    6135
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.4300
_cell_measurement_theta_min      3.8065
_cell_volume                     3708.3(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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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   24.00  102.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000    0.0000 39

  2 omega   69.00  103.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000 -120.0000 17

  3 omega   74.00  110.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000  -90.0000 18

  4 omega   49.00  115.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000   30.0000 33

  5 omega   37.00   75.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000    0.0000 19

  6 omega   36.00   62.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 13

  7 omega   37.00   63.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   30.0000 13

  8 omega   95.00  157.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  -90.0000 31

  9 omega   37.00   69.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   60.0000 16

 10 omega   92.00  154.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000    0.0000 31

 11 omega   42.00   72.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -30.0000 15

 12 omega   93.00  127.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000   30.0000 17

 13 omega   38.00  128.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000  -60.0000 45

 14 omega   89.00  149.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  150.0000 30

 15 omega   45.00   73.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  150.0000 14

 16 omega   50.00   76.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  120.0000 13

 17 omega   39.00   73.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -180.0000 17
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0558567000
_diffrn_orient_matrix_UB_12      0.0505085000
_diffrn_orient_matrix_UB_13      -0.0636798000
_diffrn_orient_matrix_UB_21      -0.0840824000
_diffrn_orient_matrix_UB_22      0.0022504000
_diffrn_orient_matrix_UB_23      0.0269682000
_diffrn_orient_matrix_UB_31      0.0245907000
_diffrn_orient_matrix_UB_32      0.1228592000
_diffrn_orient_matrix_UB_33      0.0257307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17525
_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         74.601
_diffrn_reflns_theta_min         4.237
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.820
_exptl_absorpt_correction_T_max  0.450
_exptl_absorpt_correction_T_min  0.082
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.4369
_exptl_crystal_size_mid          0.2258
_exptl_crystal_size_min          0.1735
_refine_diff_density_max         1.373
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0652P)^2^+2.0127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6580
_reflns_number_total             7406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           5I
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_original_formula_sum        'C42.50 H49 Fe I P2'
_cod_database_code               7035839
_nottingham_internal_coll_name   FEACLW
_nottingham_internal_coll_number 10407
_nottingham_internal_coll_client AC/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time 3.0000
_nottingham_internal_coll_frame_width 2.0000
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   22/6/2011
_nottingham_internal_process_date 22/06/2011
_nottingham_internal_process_user WL
_nottingham_internal_solution_date 06/01/2012
_nottingham_internal_solution_user AC
_nottingham_internal_refinement_date 06/05/2015
_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         'C41.5 H49 Fe I P2'
_chemical_oxdiff_usercomment
'FEACLW #10407 IN FOMBLIN FILM ON MICROMOUNT FOR AC/STL'
_reflns_odcompleteness_completeness 99.86
_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
 C46-C41 \\sim C42-C41
 with sigma of 0.02
 C46-C45 \\sim C43-C42
 with sigma of 0.02
 C45-C44 \\sim C44-C43
 with sigma of 0.02
 C46-C40 \\sim C40-C42
 with sigma of 0.02
 C45-C41 \\sim C41-C43
 with sigma of 0.02
 C46-C44 \\sim C44-C42
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C40, C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C41(0.5) C42(0.5) H42(0.5)
 C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5) C46(0.5) H46(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),
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
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              33614
_olex2_submission_special_instructions 'No special instructions were received'