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_7035831
_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 Cl Fe P2'
_chemical_formula_sum            'C39 H45 Cl Fe P2'
_chemical_formula_weight         666.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.390(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   43.9941(14)
_cell_length_b                   11.9191(5)
_cell_length_c                   26.0793(13)
_cell_measurement_reflns_used    7802
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      90(2)
_cell_measurement_theta_min      3.92
_cell_volume                     13561.6(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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 0.971
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details
;
  1 omega -107.00  -24.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  -77.0000   60.0000 83

  2 omega  -98.00   -3.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  125.0000 -180.0000 95

  3 omega   44.00   70.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127   38.0000 -180.0000 26

  4 omega   42.00   70.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 28

  5 omega   47.00  118.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000  -90.0000 71

  6 omega   84.00  119.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000   30.0000 35

  7 omega  128.00  153.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  -30.0000 25

  8 omega   83.00  124.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  -30.0000 41

  9 omega   48.00   76.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -180.0000 28

 10 omega   76.00  147.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   77.0000   30.0000 71

 11 omega   44.00   73.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   90.0000 29

 12 omega   89.00  114.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000  -60.0000 25

 13 omega   85.00  132.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000    0.0000 47

 14 omega   89.00  153.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  120.0000 64
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0035110000
_diffrn_orient_matrix_UB_12      0.1405010000
_diffrn_orient_matrix_UB_13      0.0258016000
_diffrn_orient_matrix_UB_21      -0.0320306000
_diffrn_orient_matrix_UB_22      -0.0221006000
_diffrn_orient_matrix_UB_23      0.0124011000
_diffrn_orient_matrix_UB_31      0.0144703000
_diffrn_orient_matrix_UB_32      0.0039227000
_diffrn_orient_matrix_UB_33      0.0522531000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.1789
_diffrn_reflns_laue_measured_fraction_full 0.971
_diffrn_reflns_laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27205
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.633
_diffrn_reflns_theta_min         3.844
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.372
_exptl_absorpt_correction_T_max  1.013
_exptl_absorpt_correction_T_min  0.534
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
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    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.1788
_exptl_crystal_size_mid          0.1459
_exptl_crystal_size_min          0.0184
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.737
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         13077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0534
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8509
_reflns_number_total             13077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00704f2.cif
_cod_data_source_block           5Cl
_cod_depositor_comments
'Adding full bibliography for 7035824--7035849.cif.'
_cod_database_code               7035831
_nottingham_internal_coll_name   FEACLJ
_nottingham_internal_coll_number 9778
_nottingham_internal_coll_client AC/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '35 and 140s'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_user   wl
_nottingham_internal_coll_date   3/2/2011
_nottingham_internal_process_date 04/02/2011
_nottingham_internal_process_user wl
_nottingham_internal_solution_date 4/2/2011
_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         'C39 H45 Cl Fe P2'
_chemical_oxdiff_usercomment
'FEACLJ #9778 IN FOMBLIN FILM ON MICROMOUNT FOR AC/STL'
_reflns_odcompleteness_completeness 89.36
_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), C40(H40A,H40B), C41(H41A,H41B)
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), C29(H29), C31(H31),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C69(H69), C70(H70)
2.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), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C),
 C78(H78A,H78B,H78C)
;
_shelx_res_checksum              6306
_olex2_submission_special_instructions 'No special instructions were received'