#------------------------------------------------------------------------------
#$Date: 2017-04-26 05:28:51 +0300 (Wed, 26 Apr 2017) $
#$Revision: 195771 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/28/7042805.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7042805
loop_
_publ_author_name
'Hitzel, Sandra'
'Färber, Christian'
'Bruhn, Clemens'
'Siemeling, Ulrich'
_publ_section_title
;
 Phosphido complexes derived from 1,1’-ferrocenediyl-bridged
 secondary diphosphines
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00941K
_journal_year                    2017
_chemical_formula_moiety         'C18 H28 Fe P2'
_chemical_formula_sum            'C18 H28 Fe P2'
_chemical_formula_weight         362.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                65.070(9)
_cell_angle_beta                 80.485(10)
_cell_angle_gamma                78.753(10)
_cell_formula_units_Z            1
_cell_length_a                   5.9610(8)
_cell_length_b                   8.9856(11)
_cell_length_c                   9.7083(12)
_cell_measurement_reflns_used    4961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.33
_cell_volume                     460.48(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      ' 141 frames, detector distance = 135 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3222
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.324
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.9552
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.58 (Stoe & Cie. 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.595
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0385
_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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1511
_reflns_number_total             1601
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00941k2.cif
_cod_data_source_block           i1049
_cod_database_code               7042805
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.917
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.4308(4) 0.5979(3) 0.1621(3) 0.0256(5) Uani 1 1 d . . .
C2 C 0.3579(4) 0.4376(3) 0.2213(3) 0.0274(6) Uani 1 1 d . . .
H2A H 0.2056 0.4142 0.2589 0.033 Uiso 1 1 calc R U .
C3 C 0.5534(5) 0.3188(3) 0.2144(3) 0.0294(6) Uani 1 1 d . . .
H3A H 0.5531 0.2033 0.2463 0.035 Uiso 1 1 calc R U .
C4 C 0.7473(4) 0.4039(3) 0.1516(3) 0.0286(6) Uani 1 1 d . . .
H4A H 0.8996 0.3552 0.1336 0.034 Uiso 1 1 calc R U .
C5 C 0.6743(4) 0.5751(3) 0.1199(3) 0.0254(5) Uani 1 1 d . . .
H5A H 0.7701 0.6598 0.0781 0.031 Uiso 1 1 calc R U .
C6 C 0.2673(4) 0.8288(3) 0.3057(3) 0.0237(5) Uani 1 1 d . . .
C7 C 0.1526(5) 0.6978(3) 0.4466(3) 0.0337(6) Uani 1 1 d . . .
H7A H -0.0083 0.7047 0.4316 0.040 Uiso 1 1 calc R U .
H7B H 0.1598 0.7182 0.5372 0.040 Uiso 1 1 calc R U .
H7C H 0.2334 0.5870 0.4606 0.040 Uiso 1 1 calc R U .
C8 C 0.1333(5) 1.0035(3) 0.2773(3) 0.0332(6) Uani 1 1 d . . .
H8A H 0.1358 1.0288 0.3658 0.040 Uiso 1 1 calc R U .
H8B H -0.0261 1.0063 0.2619 0.040 Uiso 1 1 calc R U .
H8C H 0.2053 1.0859 0.1863 0.040 Uiso 1 1 calc R U .
C9 C 0.5173(5) 0.8227(3) 0.3290(3) 0.0301(6) Uani 1 1 d . . .
H9A H 0.6008 0.7119 0.3463 0.036 Uiso 1 1 calc R U .
H9B H 0.5217 0.8472 0.4177 0.036 Uiso 1 1 calc R U .
H9C H 0.5895 0.9050 0.2380 0.036 Uiso 1 1 calc R U .
P1 P 0.24192(18) 0.79144(11) 0.13292(9) 0.0454(3) Uani 1 1 d . . .
H1 H 0.333(7) 0.845(5) 0.086(5) 0.055 Uiso 1 1 d . U .
Fe1 Fe 0.5000 0.5000 0.0000 0.0218(3) Uani 1 2 d S . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C5 106.8(2) . .
C2 C1 P1 125.2(2) . .
C5 C1 P1 127.83(19) . .
C2 C1 Fe1 69.46(13) . .
C5 C1 Fe1 69.46(13) . .
P1 C1 Fe1 122.21(13) . .
C3 C2 C1 108.6(2) . .
C3 C2 Fe1 69.89(13) . .
C1 C2 Fe1 69.69(13) . .
C3 C2 H2A 125.7 . .
C1 C2 H2A 125.7 . .
Fe1 C2 H2A 126.3 . .
C4 C3 C2 108.0(2) . .
C4 C3 Fe1 69.75(14) . .
C2 C3 Fe1 69.36(14) . .
C4 C3 H3A 126.0 . .
C2 C3 H3A 126.0 . .
Fe1 C3 H3A 126.5 . .
C3 C4 C5 108.2(2) . .
C3 C4 Fe1 69.95(14) . .
C5 C4 Fe1 69.63(14) . .
C3 C4 H4A 125.9 . .
C5 C4 H4A 125.9 . .
Fe1 C4 H4A 126.1 . .
C4 C5 C1 108.5(2) . .
C4 C5 Fe1 69.78(13) . .
C1 C5 Fe1 69.53(13) . .
C4 C5 H5A 125.8 . .
C1 C5 H5A 125.8 . .
Fe1 C5 H5A 126.5 . .
C9 C6 C7 110.1(2) . .
C9 C6 C8 110.1(2) . .
C7 C6 C8 109.9(2) . .
C9 C6 P1 112.39(17) . .
C7 C6 P1 108.59(16) . .
C8 C6 P1 105.57(17) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C1 P1 C6 103.34(11) . .
C1 P1 H1 94(3) . .
C6 P1 H1 92(3) . .
C2 Fe1 C2 180.00(7) 2_665 .
C2 Fe1 C5 68.31(10) 2_665 2_665
C2 Fe1 C5 111.69(10) . 2_665
C2 Fe1 C5 111.69(10) 2_665 .
C2 Fe1 C5 68.31(10) . .
C5 Fe1 C5 180.0 2_665 .
C2 Fe1 C1 40.85(9) 2_665 2_665
C2 Fe1 C1 139.15(9) . 2_665
C5 Fe1 C1 41.01(10) 2_665 2_665
C5 Fe1 C1 138.99(10) . 2_665
C2 Fe1 C1 139.15(9) 2_665 .
C2 Fe1 C1 40.85(9) . .
C5 Fe1 C1 138.99(10) 2_665 .
C5 Fe1 C1 41.01(10) . .
C1 Fe1 C1 180.0 2_665 .
C2 Fe1 C4 111.76(10) 2_665 .
C2 Fe1 C4 68.24(10) . .
C5 Fe1 C4 139.42(10) 2_665 .
C5 Fe1 C4 40.58(10) . .
C1 Fe1 C4 111.13(10) 2_665 .
C1 Fe1 C4 68.87(10) . .
C2 Fe1 C4 68.24(10) 2_665 2_665
C2 Fe1 C4 111.76(10) . 2_665
C5 Fe1 C4 40.58(10) 2_665 2_665
C5 Fe1 C4 139.42(10) . 2_665
C1 Fe1 C4 68.87(10) 2_665 2_665
C1 Fe1 C4 111.13(10) . 2_665
C4 Fe1 C4 180.0 . 2_665
C2 Fe1 C3 40.75(11) 2_665 2_665
C2 Fe1 C3 139.25(11) . 2_665
C5 Fe1 C3 68.12(10) 2_665 2_665
C5 Fe1 C3 111.88(10) . 2_665
C1 Fe1 C3 68.84(10) 2_665 2_665
C1 Fe1 C3 111.16(10) . 2_665
C4 Fe1 C3 139.70(10) . 2_665
C4 Fe1 C3 40.30(10) 2_665 2_665
C2 Fe1 C3 139.25(11) 2_665 .
C2 Fe1 C3 40.75(11) . .
C5 Fe1 C3 111.88(10) 2_665 .
C5 Fe1 C3 68.12(10) . .
C1 Fe1 C3 111.16(10) 2_665 .
C1 Fe1 C3 68.84(10) . .
C4 Fe1 C3 40.30(10) . .
C4 Fe1 C3 139.70(10) 2_665 .
C3 Fe1 C3 180.0 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.434(3) .
C1 C5 1.440(4) .
C1 P1 1.816(3) .
C1 Fe1 2.056(2) .
C2 C3 1.432(4) .
C2 Fe1 2.053(2) .
C2 H2A 0.9500 .
C3 C4 1.419(4) .
C3 Fe1 2.060(2) .
C3 H3A 0.9500 .
C4 C5 1.426(4) .
C4 Fe1 2.058(2) .
C4 H4A 0.9500 .
C5 Fe1 2.056(2) .
C5 H5A 0.9500 .
C6 C9 1.531(3) .
C6 C7 1.540(3) .
C6 C8 1.548(4) .
C6 P1 1.878(2) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
P1 H1 0.76(4) .
Fe1 C2 2.053(2) 2_665
Fe1 C5 2.056(2) 2_665
Fe1 C1 2.056(2) 2_665
Fe1 C4 2.058(2) 2_665
Fe1 C3 2.060(2) 2_665
