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#$Date: 2025-04-05 06:21:40 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298939 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/76/7717648.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_7717648
loop_
_publ_author_name
'Landrini, Martina'
'Navarro, Miquel'
'Campos, Jesús'
'Rocchigiani, Luca'
_publ_section_title
;
 Enhanced reactivity of cationic Au(μ-H)₂MCp₂
 complexes (M = Mo and W) enabled by bulky tris-biaryl phosphines.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              898
_journal_page_last               902
_journal_paper_doi               10.1039/d4dt03150d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C20 H20 Ag2 F12 N4 Sb2'
_chemical_formula_weight         1003.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6055(9)
_cell_length_b                   10.8282(5)
_cell_length_c                   12.7008(5)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.11
_cell_volume                     2971.3(2)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20730
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         3.109
_diffrn_source                   'IuS 3.0 Microfocus Source'
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.481
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0469
_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/[σ²(Fo²)+(0.0785P)²+18.3209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1628
_reflns_number_total             1939
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03150d2.cif
_cod_data_source_block           jcm15023
_cod_depositor_comments
'Adding full bibliography for 7717648--7717652.cif.'
_cod_database_code               7717648
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.5000 0.5000 0.36920(5) 0.0358(2) Uani 1 2 d S T P . .
Sb1 Sb 0.63513(3) 0.78542(5) 0.5000 0.0426(2) Uani 1 2 d S T P . .
F4 F 0.5676(3) 0.8927(6) 0.5000 0.0709(19) Uani 1 2 d S T P . .
F2 F 0.7008(3) 0.6743(7) 0.5000 0.085(2) Uani 1 2 d S T P . .
F3 F 0.5960(3) 0.6919(5) 0.3969(5) 0.0850(17) Uani 1 1 d . . . . .
F1 F 0.6737(3) 0.8812(6) 0.6029(5) 0.0845(16) Uani 1 1 d . . . . .
N1 N 0.5697(3) 0.3648(6) 0.3645(4) 0.0469(12) Uani 1 1 d . . . . .
C1 C 0.6300(4) 0.3972(9) 0.3603(7) 0.0600(19) Uani 1 1 d . . . . .
H1 H 0.6411 0.4821 0.3616 0.072 Uiso 1 1 calc R U . . .
C5 C 0.5566(5) 0.2450(8) 0.3615(7) 0.063(2) Uani 1 1 d . . . . .
H5 H 0.5143 0.2209 0.3637 0.075 Uiso 1 1 calc R U . . .
C2 C 0.6757(4) 0.3088(11) 0.3539(8) 0.078(3) Uani 1 1 d . . . . .
H2 H 0.7178 0.3337 0.3498 0.094 Uiso 1 1 calc R U . . .
C4 C 0.6001(5) 0.1553(9) 0.3553(8) 0.075(2) Uani 1 1 d . . . . .
H4 H 0.5884 0.0708 0.3524 0.090 Uiso 1 1 calc R U . . .
C3 C 0.6619(5) 0.1890(10) 0.3534(8) 0.074(3) Uani 1 1 d . . . . .
H3 H 0.6936 0.1282 0.3518 0.089 Uiso 1 1 calc R U . . .
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_publ_flag
N1 Ag1 N1 176.8(3) . 2_665 ?
N1 Ag1 Ag1 88.38(14) . 7_545 ?
N1 Ag1 Ag1 88.38(14) 2_665 7_545 ?
N1 Ag1 Ag1 91.62(14) . 9_666 ?
N1 Ag1 Ag1 91.62(14) 2_665 9_666 ?
Ag1 Ag1 Ag1 180.0 7_545 9_666 ?
F3 Sb1 F3 89.6(4) . 10_556 ?
F3 Sb1 F2 89.7(3) . . ?
F3 Sb1 F2 89.7(3) 10_556 . ?
F3 Sb1 F1 90.7(3) . 10_556 ?
F3 Sb1 F1 179.2(3) 10_556 10_556 ?
F2 Sb1 F1 91.1(3) . 10_556 ?
F3 Sb1 F1 179.2(3) . . ?
F3 Sb1 F1 90.7(3) 10_556 . ?
F2 Sb1 F1 91.1(3) . . ?
F1 Sb1 F1 89.0(4) 10_556 . ?
F3 Sb1 F4 89.1(2) . . ?
F3 Sb1 F4 89.1(2) 10_556 . ?
F2 Sb1 F4 178.2(3) . . ?
F1 Sb1 F4 90.2(3) 10_556 . ?
F1 Sb1 F4 90.2(3) . . ?
C5 N1 C1 117.4(7) . . ?
C5 N1 Ag1 121.8(6) . . ?
C1 N1 Ag1 120.8(6) . . ?
N1 C1 C2 120.8(9) . . ?
N1 C5 C4 123.6(9) . . ?
C3 C2 C1 121.1(10) . . ?
C5 C4 C3 118.8(10) . . ?
C2 C3 C4 118.2(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.102(6) . ?
Ag1 N1 2.102(6) 2_665 ?
Ag1 Ag1 3.0279(12) 7_545 ?
Ag1 Ag1 3.3225(12) 9_666 ?
Sb1 F3 1.859(5) . ?
Sb1 F3 1.859(5) 10_556 ?
Sb1 F2 1.860(7) . ?
Sb1 F1 1.865(5) 10_556 ?
Sb1 F1 1.865(5) . ?
Sb1 F4 1.865(6) . ?
N1 C5 1.329(11) . ?
N1 C1 1.350(10) . ?
C1 C2 1.377(13) . ?
C5 C4 1.353(13) . ?
C2 C3 1.331(15) . ?
C4 C3 1.384(15) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -0.6(12) . . . . ?
Ag1 N1 C1 C2 -178.0(7) . . . . ?
C1 N1 C5 C4 0.6(12) . . . . ?
Ag1 N1 C5 C4 178.0(7) . . . . ?
N1 C1 C2 C3 -1.0(16) . . . . ?
N1 C5 C4 C3 0.8(15) . . . . ?
C1 C2 C3 C4 2.5(16) . . . . ?
C5 C4 C3 C2 -2.4(16) . . . . ?
