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#$Date: 2022-10-21 01:36:47 +0300 (Fri, 21 Oct 2022) $
#$Revision: 278672 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/56/7245691.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_7245691
loop_
_publ_author_name
'Morales-Morales, David'
'Juarez-Garrido, Hugo'
'German-Acacio, Juan Manuel'
'Jaime-Adán, Everardo'
'Barroso-Flores, Joaquín'
'Lara, Victor Hugo'
'Reyes-Martinez, Reyna'
'Toscano, Ruben Alfredo'
'Hernandez Ortega, Simon'
_publ_section_title
;
 Synthesis of a Series of Pd(II) Complexes of the Type
 [Pd(1,10-phen)(SRF)2]·Solvent. An Interesting Case of
 Solvatomorphism
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01319C
_journal_year                    2022
_chemical_formula_sum            'C30 H13 Br F10 N2 Pd S2'
_chemical_formula_weight         841.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-17 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.053(2)
_cell_angle_beta                 79.641(2)
_cell_angle_gamma                76.947(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3031(12)
_cell_length_b                   11.7857(15)
_cell_length_c                   14.3880(18)
_cell_measurement_reflns_used    8645
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.398
_cell_measurement_theta_min      2.259
_cell_volume                     1407.8(3)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer 01-670'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12704
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.545
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0302
_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)+(0.0348P)²+1.5689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4733
_reflns_number_total             5160
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01319c2.cif
_cod_data_source_block           Compound-5
_cod_database_code               7245691
_shelx_shelxl_version_number     2018/3
_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   0.407
_shelx_estimated_absorpt_t_max   0.675
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.19876(2) 0.41405(2) 0.17987(2) 0.01858(8) Uani 1 1 d . . . . .
S1 S 0.37927(9) 0.25158(8) 0.24922(6) 0.03001(19) Uani 1 1 d . . . . .
S2 S 0.05167(8) 0.39212(7) 0.32925(5) 0.02306(16) Uani 1 1 d . . . . .
F1 F 0.1746(2) 0.06493(18) 0.35768(15) 0.0378(5) Uani 1 1 d . . . . .
F2 F 0.1406(2) -0.0717(2) 0.55613(17) 0.0485(6) Uani 1 1 d . . . . .
F3 F 0.2860(2) -0.0370(2) 0.68736(14) 0.0492(6) Uani 1 1 d . . . . .
F4 F 0.4711(2) 0.1334(2) 0.61699(15) 0.0460(5) Uani 1 1 d . . . . .
F5 F 0.5098(2) 0.26778(18) 0.41918(15) 0.0372(5) Uani 1 1 d . . . . .
F6 F 0.0558(2) 0.26735(17) 0.55119(13) 0.0340(4) Uani 1 1 d . . . . .
F7 F 0.1927(2) 0.3147(2) 0.67620(14) 0.0452(5) Uani 1 1 d . . . . .
F8 F 0.3443(2) 0.5095(2) 0.60528(17) 0.0505(6) Uani 1 1 d . . . . .
F9 F 0.3686(2) 0.6475(2) 0.40369(18) 0.0467(5) Uani 1 1 d . . . . .
F10 F 0.2407(2) 0.59626(17) 0.27537(13) 0.0332(4) Uani 1 1 d . . . . .
C1 C 0.3436(3) 0.1715(3) 0.3802(2) 0.0220(6) Uani 1 1 d . . . . .
C2 C 0.2499(3) 0.0839(3) 0.4197(2) 0.0266(7) Uani 1 1 d . . . . .
C3 C 0.2308(3) 0.0131(3) 0.5215(2) 0.0305(7) Uani 1 1 d . . . . .
C4 C 0.3052(4) 0.0303(3) 0.5878(2) 0.0311(7) Uani 1 1 d . . . . .
C5 C 0.3989(4) 0.1157(3) 0.5523(2) 0.0302(7) Uani 1 1 d . . . . .
C6 C 0.4170(3) 0.1850(3) 0.4499(2) 0.0258(7) Uani 1 1 d . . . . .
C7 C 0.1440(3) 0.4284(3) 0.4076(2) 0.0232(6) Uani 1 1 d . . . . .
C8 C 0.1338(3) 0.3617(3) 0.5114(2) 0.0269(7) Uani 1 1 d . . . . .
C9 C 0.2017(4) 0.3865(3) 0.5771(2) 0.0327(8) Uani 1 1 d . . . . .
C10 C 0.2803(4) 0.4830(3) 0.5411(3) 0.0353(8) Uani 1 1 d . . . . .
C11 C 0.2922(4) 0.5526(3) 0.4397(3) 0.0332(7) Uani 1 1 d . . . . .
C12 C 0.2257(3) 0.5257(3) 0.3741(2) 0.0279(7) Uani 1 1 d . . . . .
N13 N 0.3085(3) 0.4404(2) 0.03520(17) 0.0197(5) Uani 1 1 d . . . . .
C14 C 0.4312(3) 0.3730(3) 0.0074(2) 0.0238(6) Uani 1 1 d . . . . .
H14 H 0.480717 0.303643 0.058403 0.029 Uiso 1 1 calc R U . . .
C15 C 0.4900(3) 0.4000(3) -0.0933(2) 0.0257(6) Uani 1 1 d . . . . .
H15 H 0.578372 0.349907 -0.110065 0.031 Uiso 1 1 calc R U . . .
C16 C 0.4196(3) 0.4997(3) -0.1686(2) 0.0266(7) Uani 1 1 d . . . . .
H16 H 0.459019 0.519259 -0.237628 0.032 Uiso 1 1 calc R U . . .
C17 C 0.2067(3) 0.6766(3) -0.2146(2) 0.0273(7) Uani 1 1 d . . . . .
H17 H 0.241784 0.700476 -0.284613 0.033 Uiso 1 1 calc R U . . .
C18 C 0.0799(4) 0.7420(3) -0.1849(2) 0.0279(7) Uani 1 1 d . . . . .
H18 H 0.027364 0.810960 -0.234495 0.033 Uiso 1 1 calc R U . . .
C19 C -0.1092(3) 0.7722(3) -0.0453(2) 0.0260(7) Uani 1 1 d . . . . .
H19 H -0.166862 0.841180 -0.091638 0.031 Uiso 1 1 calc R U . . .
C20 C -0.1539(3) 0.7331(3) 0.0558(2) 0.0268(7) Uani 1 1 d . . . . .
H20 H -0.242678 0.775430 0.080414 0.032 Uiso 1 1 calc R U . . .
C21 C -0.0696(3) 0.6306(3) 0.1239(2) 0.0245(6) Uani 1 1 d . . . . .
H21 H -0.103366 0.604219 0.194129 0.029 Uiso 1 1 calc R U . . .
N22 N 0.0555(3) 0.5691(2) 0.09374(18) 0.0200(5) Uani 1 1 d . . . . .
C23 C 0.2366(3) 0.5387(3) -0.0388(2) 0.0203(6) Uani 1 1 d . . . . .
C24 C 0.2889(3) 0.5719(3) -0.1420(2) 0.0232(6) Uani 1 1 d . . . . .
C25 C 0.1027(3) 0.6080(3) -0.0079(2) 0.0201(6) Uani 1 1 d . . . . .
C26 C 0.0236(3) 0.7095(3) -0.0806(2) 0.0235(6) Uani 1 1 d . . . . .
Br1 Br 0.30253(5) -0.07478(4) -0.08502(3) 0.05057(12) Uani 1 1 d . . . . .
C27 C 0.2487(4) -0.0913(3) 0.0525(3) 0.0373(8) Uani 1 1 d . . . . .
C28 C 0.1069(4) -0.1081(3) 0.0952(3) 0.0423(9) Uani 1 1 d . . . . .
H28 H 0.037435 -0.113121 0.056554 0.051 Uiso 1 1 calc R U . . .
C29 C 0.0663(5) -0.1177(4) 0.1946(3) 0.0480(10) Uani 1 1 d . . . . .
H29 H -0.031560 -0.129316 0.224462 0.058 Uiso 1 1 calc R U . . .
C30 C 0.1657(5) -0.1106(3) 0.2503(3) 0.0473(10) Uani 1 1 d . . . . .
H30 H 0.137294 -0.117880 0.318903 0.057 Uiso 1 1 calc R U . . .
C31 C 0.3076(5) -0.0928(4) 0.2070(3) 0.0485(10) Uani 1 1 d . . . . .
H31 H 0.376257 -0.086762 0.245681 0.058 Uiso 1 1 calc R U . . .
C32 C 0.3504(4) -0.0837(3) 0.1076(3) 0.0433(9) Uani 1 1 d . . . . .
H32 H 0.448409 -0.072282 0.077809 0.052 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
N13 Pd1 N22 80.07(9) . . ?
N13 Pd1 S1 90.62(7) . . ?
N22 Pd1 S1 170.57(7) . . ?
N13 Pd1 S2 172.88(7) . . ?
N22 Pd1 S2 94.23(7) . . ?
S1 Pd1 S2 95.16(3) . . ?
C1 S1 Pd1 114.52(10) . . ?
C7 S2 Pd1 108.18(10) . . ?
C6 C1 C2 115.8(3) . . ?
C6 C1 S1 121.6(2) . . ?
C2 C1 S1 122.3(2) . . ?
F1 C2 C3 117.4(3) . . ?
F1 C2 C1 119.8(3) . . ?
C3 C2 C1 122.8(3) . . ?
F2 C3 C4 119.9(3) . . ?
F2 C3 C2 120.8(3) . . ?
C4 C3 C2 119.3(3) . . ?
F3 C4 C5 120.2(3) . . ?
F3 C4 C3 119.9(3) . . ?
C5 C4 C3 120.0(3) . . ?
F4 C5 C4 120.1(3) . . ?
F4 C5 C6 120.1(3) . . ?
C4 C5 C6 119.7(3) . . ?
F5 C6 C5 117.2(3) . . ?
F5 C6 C1 120.4(3) . . ?
C5 C6 C1 122.4(3) . . ?
C8 C7 C12 115.2(3) . . ?
C8 C7 S2 120.0(2) . . ?
C12 C7 S2 124.8(2) . . ?
F6 C8 C9 117.4(3) . . ?
F6 C8 C7 119.6(3) . . ?
C9 C8 C7 122.9(3) . . ?
F7 C9 C10 120.2(3) . . ?
F7 C9 C8 119.8(3) . . ?
C10 C9 C8 120.0(3) . . ?
F8 C10 C11 120.3(3) . . ?
F8 C10 C9 120.2(3) . . ?
C11 C10 C9 119.4(3) . . ?
F9 C11 C10 119.9(3) . . ?
F9 C11 C12 119.9(3) . . ?
C10 C11 C12 120.2(3) . . ?
F10 C12 C11 118.0(3) . . ?
F10 C12 C7 119.7(3) . . ?
C11 C12 C7 122.3(3) . . ?
C14 N13 C23 118.3(2) . . ?
C14 N13 Pd1 129.0(2) . . ?
C23 N13 Pd1 112.68(19) . . ?
N13 C14 C15 122.7(3) . . ?
C16 C15 C14 119.7(3) . . ?
C15 C16 C24 119.1(3) . . ?
C18 C17 C24 121.0(3) . . ?
C17 C18 C26 121.3(3) . . ?
C20 C19 C26 119.3(3) . . ?
C19 C20 C21 120.2(3) . . ?
N22 C21 C20 122.3(3) . . ?
C21 N22 C25 118.2(2) . . ?
C21 N22 Pd1 129.3(2) . . ?
C25 N22 Pd1 112.51(18) . . ?
N13 C23 C24 122.5(3) . . ?
N13 C23 C25 117.6(2) . . ?
C24 C23 C25 119.9(3) . . ?
C23 C24 C16 117.8(3) . . ?
C23 C24 C17 118.8(3) . . ?
C16 C24 C17 123.4(3) . . ?
N22 C25 C26 122.7(3) . . ?
N22 C25 C23 117.1(2) . . ?
C26 C25 C23 120.1(3) . . ?
C25 C26 C19 117.2(3) . . ?
C25 C26 C18 118.8(3) . . ?
C19 C26 C18 123.9(3) . . ?
C28 C27 C32 120.9(4) . . ?
C28 C27 Br1 119.2(3) . . ?
C32 C27 Br1 119.9(3) . . ?
C27 C28 C29 119.5(4) . . ?
C30 C29 C28 120.4(4) . . ?
C29 C30 C31 120.0(4) . . ?
C30 C31 C32 120.4(4) . . ?
C27 C32 C31 118.9(4) . . ?
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
Pd1 N13 2.085(2) . ?
Pd1 N22 2.093(2) . ?
Pd1 S1 2.2677(8) . ?
Pd1 S2 2.2865(8) . ?
S1 C1 1.755(3) . ?
S2 C7 1.755(3) . ?
F1 C2 1.337(3) . ?
F2 C3 1.338(4) . ?
F3 C4 1.341(4) . ?
F4 C5 1.342(4) . ?
F5 C6 1.342(4) . ?
F6 C8 1.345(4) . ?
F7 C9 1.343(4) . ?
F8 C10 1.346(4) . ?
F9 C11 1.341(4) . ?
F10 C12 1.338(4) . ?
C1 C6 1.384(4) . ?
C1 C2 1.385(4) . ?
C2 C3 1.377(4) . ?
C3 C4 1.372(5) . ?
C4 C5 1.367(5) . ?
C5 C6 1.379(4) . ?
C7 C8 1.389(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.375(5) . ?
C9 C10 1.370(5) . ?
C10 C11 1.366(5) . ?
C11 C12 1.381(5) . ?
N13 C14 1.329(4) . ?
N13 C23 1.367(4) . ?
C14 C15 1.391(4) . ?
C15 C16 1.378(4) . ?
C16 C24 1.403(4) . ?
C17 C18 1.355(5) . ?
C17 C24 1.434(4) . ?
C18 C26 1.425(4) . ?
C19 C20 1.359(5) . ?
C19 C26 1.409(4) . ?
C20 C21 1.399(4) . ?
C21 N22 1.323(4) . ?
N22 C25 1.371(4) . ?
C23 C24 1.402(4) . ?
C23 C25 1.429(4) . ?
C25 C26 1.403(4) . ?
Br1 C27 1.895(4) . ?
C27 C28 1.374(5) . ?
C27 C32 1.377(5) . ?
C28 C29 1.378(6) . ?
C29 C30 1.363(6) . ?
C30 C31 1.379(6) . ?
C31 C32 1.382(6) . ?
