#------------------------------------------------------------------------------
#$Date: 2023-12-12 11:56:26 +0200 (Tue, 12 Dec 2023) $
#$Revision: 288243 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/73/1547385.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_1547385
loop_
_publ_author_name
'Nicolas Delpont'
'Imma Escofet'
'Patricia Perez-Galen'
'Dirk Spiegl'
'Mihai Raducan'
'Christophe Bour'
'Riccardo Sinisi'
'Antonio M. Echavarrena'
_publ_section_title
;
 Modular chiral gold(i) phosphite complexes
;
_journal_name_full               'Catalysis Science & Technology'
_journal_page_first              3007
_journal_page_last               3012
_journal_paper_doi               10.1039/c3cy00250k
_journal_volume                  3
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_sum            'C32 H25 Au Cl Fe P'
_chemical_formula_weight         728.76
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2861(14)
_cell_length_b                   13.2861(14)
_cell_length_c                   14.7974(15)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      2.57
_cell_volume                     2612.0(5)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33908
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    6.349
_exptl_absorpt_correction_T_max  0.5693
_exptl_absorpt_correction_T_min  0.2517
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Version 2008/1 Bruker-Nonius
Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.432
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6715
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0746P)²+2.6694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                6497
_reflns_number_total             6715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CY-003-C3CY00250K-s003.cif
_cod_data_source_block           mo_rs271p41
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 

The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      P4(1)
_cod_database_code               1547385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C8 C 0.6321(4) 0.8614(4) 1.1383(3) 0.0300(10) Uani 1 1 d . . .
H8 H 0.6575 0.9215 1.1643 0.036 Uiso 1 1 calc R . .
C10 C 0.6580(3) 0.6903(3) 1.0884(3) 0.0236(8) Uani 1 1 d . . .
C9 C 0.6929(3) 0.7793(4) 1.1303(3) 0.0291(9) Uani 1 1 d . . .
H9 H 0.7597 0.7819 1.1532 0.035 Uiso 1 1 calc R . .
C6 C 0.4924(3) 0.7720(3) 1.0671(3) 0.0200(7) Uani 1 1 d . . .
C12 C 0.5236(3) 0.5978(3) 1.0108(3) 0.0214(8) Uani 1 1 d . . .
H12 H 0.4570 0.5940 0.9879 0.026 Uiso 1 1 calc R . .
C3 C 0.3114(3) 0.7015(3) 1.0767(3) 0.0234(8) Uani 1 1 d . . .
H3 H 0.3197 0.6618 1.1336 0.028 Uiso 1 1 calc R . .
C5 C 0.2393(3) 0.7735(3) 0.9498(3) 0.0243(8) Uani 1 1 d . . .
H5 H 0.1896 0.7916 0.9018 0.029 Uiso 1 1 calc R . .
C1 C 0.3411(3) 0.8101(3) 0.9567(3) 0.0187(7) Uani 1 1 d . . .
C2 C 0.3865(3) 0.7645(3) 1.0366(3) 0.0206(7) Uani 1 1 d . . .
C19 C 0.1850(4) 0.9821(4) 1.0624(4) 0.0350(11) Uani 1 1 d . . .
H19 H 0.1616 1.0164 1.0060 0.042 Uiso 1 1 calc R . .
C11 C 0.5566(3) 0.6866(3) 1.0550(3) 0.0196(7) Uani 1 1 d . . .
C7 C 0.5310(4) 0.8575(3) 1.1080(3) 0.0262(9) Uani 1 1 d . . .
H7 H 0.4889 0.9146 1.1159 0.031 Uiso 1 1 calc R . .
C16 C 0.2815(4) 0.9334(4) 1.1842(3) 0.0369(11) Uani 1 1 d . . .
H16 H 0.3386 0.9270 1.2279 0.044 Uiso 1 1 calc R . .
C17 C 0.1896(5) 0.8812(4) 1.1885(4) 0.0394(13) Uani 1 1 d . . .
H17 H 0.1704 0.8312 1.2359 0.047 Uiso 1 1 calc R . .
C13 C 0.5876(4) 0.5171(3) 1.0009(3) 0.0265(9) Uani 1 1 d . . .
H13 H 0.5650 0.4589 0.9695 0.032 Uiso 1 1 calc R . .
C14 C 0.6848(4) 0.5192(4) 1.0360(4) 0.0326(10) Uani 1 1 d . . .
H14 H 0.7271 0.4620 1.0297 0.039 Uiso 1 1 calc R . .
C15 C 0.7202(3) 0.6039(4) 1.0799(4) 0.0296(9) Uani 1 1 d . . .
H15 H 0.7863 0.6044 1.1044 0.036 Uiso 1 1 calc R . .
C20 C 0.2792(4) 0.9969(4) 1.1059(4) 0.0348(11) Uani 1 1 d . . .
H20 H 0.3342 1.0428 1.0853 0.042 Uiso 1 1 calc R . .
C18 C 0.1286(4) 0.9113(4) 1.1149(4) 0.0402(13) Uani 1 1 d . . .
H18 H 0.0590 0.8868 1.1015 0.048 Uiso 1 1 calc R . .
C4 C 0.2219(3) 0.7072(3) 1.0243(4) 0.0277(9) Uani 1 1 d . . .
H4 H 0.1573 0.6715 1.0378 0.033 Uiso 1 1 calc R . .
C21 C 0.4141(3) 0.8223(3) 0.7743(3) 0.0196(7) Uani 1 1 d . . .
C22 C 0.4023(4) 0.7192(3) 0.7680(3) 0.0296(10) Uani 1 1 d . . .
H22 H 0.3822 0.6817 0.8196 0.036 Uiso 1 1 calc R . .
C26 C 0.4438(4) 0.8755(4) 0.6969(3) 0.0317(10) Uani 1 1 d . . .
H26 H 0.4537 0.9462 0.7005 0.038 Uiso 1 1 calc R . .
C27 C 0.3077(3) 0.9889(3) 0.8522(3) 0.0234(8) Uani 1 1 d . . .
C29 C 0.2468(5) 1.1579(4) 0.8760(4) 0.0449(14) Uani 1 1 d . . .
H29 H 0.2561 1.2234 0.9002 0.054 Uiso 1 1 calc R . .
C28 C 0.3207(4) 1.0856(3) 0.8872(4) 0.0330(10) Uani 1 1 d . . .
H28 H 0.3806 1.1019 0.9189 0.040 Uiso 1 1 calc R . .
C32 C 0.2202(3) 0.9662(3) 0.8027(3) 0.0261(9) Uani 1 1 d . . .
H32 H 0.2112 0.9014 0.7769 0.031 Uiso 1 1 calc R . .
Au1 Au 0.548210(11) 0.958483(11) 0.916393(15) 0.02319(6) Uani 1 1 d . . .
Fe1 Fe 0.26088(5) 0.84826(5) 1.06901(4) 0.02243(12) Uani 1 1 d . . .
P1 P 0.39981(8) 0.89302(7) 0.87821(7) 0.01913(19) Uani 1 1 d . . .
Cl1 Cl 0.70234(9) 1.02987(10) 0.94039(9) 0.0359(3) Uani 1 1 d . . .
C23 C 0.4197(5) 0.6702(4) 0.6864(4) 0.0373(12) Uani 1 1 d . . .
H23 H 0.4133 0.5991 0.6829 0.045 Uiso 1 1 calc R . .
C24 C 0.4462(4) 0.7245(4) 0.6106(4) 0.0358(11) Uani 1 1 d . . .
H24 H 0.4559 0.6908 0.5546 0.043 Uiso 1 1 calc R . .
C25 C 0.4588(4) 0.8272(4) 0.6155(4) 0.0374(11) Uani 1 1 d . . .
H25 H 0.4776 0.8645 0.5634 0.045 Uiso 1 1 calc R . .
C31 C 0.1463(4) 1.0408(4) 0.7921(4) 0.0387(12) Uani 1 1 d . . .
H31 H 0.0868 1.0262 0.7590 0.046 Uiso 1 1 calc R . .
C30 C 0.1593(5) 1.1349(4) 0.8294(4) 0.0478(16) Uani 1 1 d . . .
H30 H 0.1080 1.1843 0.8231 0.057 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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'
Au Au -2.0133 8.8022 '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
C9 C8 C7 120.4(4) . .
C9 C10 C15 121.5(4) . .
C9 C10 C11 119.2(4) . .
C15 C10 C11 119.2(4) . .
C8 C9 C10 120.8(4) . .
C7 C6 C11 119.0(4) . .
C7 C6 C2 122.7(4) . .
C11 C6 C2 118.3(3) . .
C13 C12 C11 120.5(4) . .
C4 C3 C2 109.1(4) . .
C4 C3 Fe1 69.4(3) . .
C2 C3 Fe1 69.6(2) . .
C4 C5 C1 107.8(4) . .
C4 C5 Fe1 70.0(3) . .
C1 C5 Fe1 69.1(3) . .
C5 C1 C2 107.7(4) . .
C5 C1 P1 125.0(3) . .
C2 C1 P1 127.2(3) . .
C5 C1 Fe1 69.5(3) . .
C2 C1 Fe1 70.0(2) . .
P1 C1 Fe1 127.4(2) . .
C3 C2 C1 106.9(4) . .
C3 C2 C6 125.2(4) . .
C1 C2 C6 127.6(4) . .
C3 C2 Fe1 69.9(2) . .
C1 C2 Fe1 68.3(2) . .
C6 C2 Fe1 131.5(3) . .
C20 C19 C18 107.8(5) . .
C20 C19 Fe1 70.4(3) . .
C18 C19 Fe1 70.2(3) . .
C12 C11 C6 122.3(4) . .
C12 C11 C10 118.5(4) . .
C6 C11 C10 119.3(4) . .
C6 C7 C8 121.3(4) . .
C17 C16 C20 108.0(5) . .
C17 C16 Fe1 69.6(3) . .
C20 C16 Fe1 69.6(3) . .
C16 C17 C18 108.9(5) . .
C16 C17 Fe1 70.5(3) . .
C18 C17 Fe1 70.2(3) . .
C12 C13 C14 121.2(4) . .
C15 C14 C13 120.5(4) . .
C14 C15 C10 120.1(4) . .
C19 C20 C16 107.6(5) . .
C19 C20 Fe1 69.2(3) . .
C16 C20 Fe1 69.7(3) . .
C17 C18 C19 107.6(5) . .
C17 C18 Fe1 69.5(3) . .
C19 C18 Fe1 69.0(3) . .
C3 C4 C5 108.5(4) . .
C3 C4 Fe1 70.3(3) . .
C5 C4 Fe1 69.2(3) . .
C22 C21 C26 118.4(4) . .
C22 C21 P1 124.0(4) . .
C26 C21 P1 117.5(3) . .
C21 C22 C23 120.2(5) . .
C25 C26 C21 121.3(4) . .
C28 C27 C32 119.5(4) . .
C28 C27 P1 119.1(4) . .
C32 C27 P1 121.3(3) . .
C30 C29 C28 120.1(5) . .
C29 C28 C27 120.5(6) . .
C31 C32 C27 119.0(5) . .
P1 Au1 Cl1 174.16(5) . .
C1 Fe1 C5 41.33(16) . .
C1 Fe1 C19 115.8(2) . .
C5 Fe1 C19 108.2(2) . .
C1 Fe1 C17 175.1(2) . .
C5 Fe1 C17 141.4(2) . .
C19 Fe1 C17 68.2(2) . .
C1 Fe1 C4 69.06(18) . .
C5 Fe1 C4 40.85(18) . .
C19 Fe1 C4 130.8(2) . .
C17 Fe1 C4 110.8(2) . .
C1 Fe1 C2 41.69(16) . .
C5 Fe1 C2 69.56(17) . .
C19 Fe1 C2 148.93(19) . .
C17 Fe1 C2 133.5(2) . .
C4 Fe1 C2 68.70(17) . .
C1 Fe1 C20 113.07(19) . .
C5 Fe1 C20 135.2(2) . .
C19 Fe1 C20 40.5(2) . .
C17 Fe1 C20 67.8(2) . .
C4 Fe1 C20 171.3(2) . .
C2 Fe1 C20 118.8(2) . .
C1 Fe1 C18 144.6(2) . .
C5 Fe1 C18 111.2(2) . .
C19 Fe1 C18 40.8(2) . .
C17 Fe1 C18 40.2(2) . .
C4 Fe1 C18 105.2(2) . .
C2 Fe1 C18 170.2(2) . .
C20 Fe1 C18 68.0(2) . .
C1 Fe1 C3 68.90(17) . .
C5 Fe1 C3 68.54(18) . .
C19 Fe1 C3 169.4(2) . .
C17 Fe1 C3 107.7(2) . .
C4 Fe1 C3 40.36(17) . .
C2 Fe1 C3 40.56(16) . .
C20 Fe1 C3 148.3(2) . .
C18 Fe1 C3 130.0(2) . .
C1 Fe1 C16 137.8(2) . .
C5 Fe1 C16 175.8(2) . .
C19 Fe1 C16 68.2(2) . .
C17 Fe1 C16 39.9(3) . .
C4 Fe1 C16 143.1(2) . .
C2 Fe1 C16 112.3(2) . .
C20 Fe1 C16 40.7(2) . .
C18 Fe1 C16 67.6(3) . .
C3 Fe1 C16 115.4(2) . .
C1 P1 C27 106.16(19) . .
C1 P1 C21 106.19(19) . .
C27 P1 C21 104.8(2) . .
C1 P1 Au1 117.63(14) . .
C27 P1 Au1 112.19(15) . .
C21 P1 Au1 108.95(14) . .
C24 C23 C22 120.2(4) . .
C25 C24 C23 120.4(5) . .
C24 C25 C26 119.4(5) . .
C30 C31 C32 120.5(6) . .
C31 C30 C29 120.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C8 C9 1.363(7) .
C8 C7 1.416(6) .
C10 C9 1.413(7) .
C10 C15 1.421(7) .
C10 C11 1.436(6) .
C6 C7 1.385(6) .
C6 C11 1.430(6) .
C6 C2 1.482(6) .
C12 C13 1.376(6) .
C12 C11 1.419(6) .
C3 C4 1.421(6) .
C3 C2 1.431(6) .
C3 Fe1 2.066(4) .
C5 C4 1.430(6) .
C5 C1 1.441(5) .
C5 Fe1 2.044(5) .
C1 C2 1.459(6) .
C1 P1 1.780(4) .
C1 Fe1 2.039(4) .
C2 Fe1 2.062(4) .
C19 C20 1.421(8) .
C19 C18 1.432(8) .
C19 Fe1 2.047(5) .
C16 C17 1.405(9) .
C16 C20 1.434(7) .
C16 Fe1 2.064(5) .
C17 C18 1.416(8) .
C17 Fe1 2.052(5) .
C13 C14 1.392(7) .
C14 C15 1.383(8) .
C20 Fe1 2.063(5) .
C18 Fe1 2.062(5) .
C4 Fe1 2.054(5) .
C21 C22 1.382(5) .
C21 C26 1.402(6) .
C21 P1 1.812(4) .
C22 C23 1.391(7) .
C26 C25 1.378(7) .
C27 C28 1.395(6) .
C27 C32 1.407(7) .
C27 P1 1.808(4) .
C29 C30 1.386(11) .
C29 C28 1.383(7) .
C32 C31 1.404(6) .
Au1 P1 2.2278(11) .
Au1 Cl1 2.2845(11) .
C23 C24 1.380(8) .
C24 C25 1.377(8) .
C31 C30 1.377(9) .
