#------------------------------------------------------------------------------
#$Date: 2022-05-20 01:52:06 +0300 (Fri, 20 May 2022) $
#$Revision: 275564 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/02/7710293.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_7710293
loop_
_publ_author_name
'Singh, Mukesh K.'
'Etcheverry-Berríos, Alvaro'
'Vallejo, Julia'
'Sanz, Sergio'
'Martínez-Lillo, José'
'Nichol, Gary S.'
'Lusby, Paul J.'
'Brechin, Euan K.'
_publ_section_title
;
 Guest-induced magnetic exchange in paramagnetic [M2L4]4+ coordination
 cages
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01385A
_journal_year                    2022
_chemical_formula_moiety         'Cl6 Re, C80 H48 N8 Pd2, 2(F6 P), 6(C2 H3 N)'
_chemical_formula_sum            'C92 H66 Cl6 F12 N14 P2 Pd2 Re'
_chemical_formula_weight         2269.22
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-08-24 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                93.695(3)
_cell_angle_beta                 99.071(3)
_cell_angle_gamma                118.328(3)
_cell_formula_units_Z            1
_cell_length_a                   12.1451(4)
_cell_length_b                   12.7786(4)
_cell_length_c                   17.3925(6)
_cell_measurement_reflns_used    11783
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.2390
_cell_measurement_theta_min      3.9660
_cell_volume                     2316.00(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  29.00   1.00   10.00    --  -41.42  57.00-150.00   97
  2  ω   -127.00 -34.00   1.00   10.00    --  -41.42 178.00-180.00   93
  3  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00  60.00   97
  4  ω     19.00 114.00   1.00   10.00    --   41.42  38.00   0.00   95
  5  ω      1.00  81.00   1.00   10.00    --   41.42 -99.00   0.00   80
  6  ω     87.00 178.00   1.00   30.00    --  111.00  45.00  60.00   91
  7  ω     40.00 125.00   1.00   30.00    --  111.00-131.00 138.00   85
  8  ω     41.00 128.00   1.00   30.00    --  111.00-138.00 -36.00   87
  9  ω     80.00 178.00   1.00   30.00    --  111.00  77.00   0.00   98
 10  ω     94.00 178.00   1.00   30.00    --  111.00 125.00-120.00   84
 11  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 120.00   95
 12  ω     87.00 178.00   1.00   30.00    --  111.00  30.00 -30.00   91
 13  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00-150.00   79
 14  ω     39.00 121.00   1.00   30.00    --  111.00-125.00   0.00   82
 15  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00 150.00   79
 16  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00 -30.00   79
 17  ω     41.00 139.00   1.00   30.00    --  111.00 -61.00 -30.00   98
 18  ω     36.00 135.00   1.00   30.00    --  111.00 -30.00  90.00   99
 19  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00 150.00   97
 20  ω   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00 -30.00  105
 21  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00-150.00   97
 22  ω   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00  60.00  105
 23  ω   -112.00 -65.00   1.00   10.00    --  -41.42-138.00 -36.00   47
 24  ω     87.00 178.00   1.00   30.00    --  111.00  30.00 -90.00   91
 25  ω     87.00 178.00   1.00   30.00    --  111.00  30.00-150.00   91
 26  ω     83.00 178.00   1.00   30.00    --  111.00  61.00-150.00   95
 27  ω     83.00 178.00   1.00   30.00    --  111.00  61.00  90.00   95
 28  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190161000
_diffrn_orient_matrix_UB_12      -0.0238428000
_diffrn_orient_matrix_UB_13      -0.0903642000
_diffrn_orient_matrix_UB_21      0.0978849000
_diffrn_orient_matrix_UB_22      -0.0451046000
_diffrn_orient_matrix_UB_23      0.0093297000
_diffrn_orient_matrix_UB_31      -0.1087299000
_diffrn_orient_matrix_UB_32      -0.1290316000
_diffrn_orient_matrix_UB_33      -0.0022176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.222
_diffrn_reflns_theta_min         3.981
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.183
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       plate
_exptl_crystal_F_000             1123
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of hexane and dichloromethane by vapour diffusion'
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.080
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.147
_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     586
_refine_ls_number_reflns         9485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0550
_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)+(0.0830P)²+4.3337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7713
_reflns_number_total             9485
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01385a2.cif
_cod_data_source_block           5
_cod_database_code               7710293
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C92 H66 Cl6 F12 N14 P2 Pd2 Re1'
_chemical_oxdiff_usercomment     '@ 120 K JV322-hexane'
_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.
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C38(H38), C11(H11), C21(H21), C25(H25), C31(H31), C33(H33),
 C13(H13), C9(H9), C1(H1), C34(H34), C30(H30), C29(H29), C14(H14), C10(H10),
 C2(H2), C36(H36), C35(H35), C23(H23), C15(H15), C22(H22), C16(H16), C3(H3)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C)
;
_olex2_date_sample_data_collection 2017-03-28
_olex2_date_sample_submission    2017-01-19
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JV322-hexane
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.669
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
Re1 Re 0.000000 0.500000 0.500000 0.02609(11) Uani 1 2 d S T P . .
Pd1 Pd 0.09807(4) 0.33638(3) 0.79642(2) 0.02257(11) Uani 1 1 d . . . . .
P1 P 0.78218(17) 0.76070(16) 0.95270(9) 0.0360(3) Uani 1 1 d . . . . .
Cl2 Cl 0.15091(17) 0.44181(17) 0.54956(11) 0.0474(4) Uani 1 1 d . . . . .
Cl1 Cl -0.15914(17) 0.33401(16) 0.54325(11) 0.0490(4) Uani 1 1 d . . . . .
Cl3 Cl 0.0521(2) 0.61878(17) 0.62392(10) 0.0505(4) Uani 1 1 d . . . . .
F6 F 0.8673(4) 0.7516(4) 1.0306(2) 0.0478(10) Uani 1 1 d . . . . .
F5 F 0.6930(5) 0.7676(4) 0.8767(2) 0.0543(11) Uani 1 1 d . . . . .
N4 N 0.0368(5) 0.8329(4) 0.2475(3) 0.0275(10) Uani 1 1 d . . . . .
N3 N 0.2368(4) 0.5043(4) 0.8421(3) 0.0264(9) Uani 1 1 d . . . . .
N1 N 0.2297(5) 0.2981(4) 0.7672(3) 0.0250(9) Uani 1 1 d . . . . .
F1 F 0.6741(5) 0.6253(5) 0.9511(4) 0.0742(16) Uani 1 1 d . . . . .
N2 N 0.0317(4) 0.6238(4) 0.1716(3) 0.0263(9) Uani 1 1 d . . . . .
F3 F 0.8872(6) 0.8914(5) 0.9524(4) 0.089(2) Uani 1 1 d . . . . .
F4 F 0.7116(6) 0.8021(6) 1.0063(3) 0.0763(17) Uani 1 1 d . . . . .
C5 C 0.2605(5) 0.3144(5) 0.6972(3) 0.0255(11) Uani 1 1 d . . . . .
H5 H 0.218665 0.343905 0.661223 0.031 Uiso 1 1 calc R . . . .
C18 C 0.0891(5) 0.5770(5) 0.2188(3) 0.0262(11) Uani 1 1 d . . . . .
H18 H 0.069123 0.563478 0.269126 0.031 Uiso 1 1 calc R . . . .
F2 F 0.8436(6) 0.7109(7) 0.8985(3) 0.0841(19) Uani 1 1 d . . . . .
C8 C 0.4188(6) 0.3510(5) 0.4565(3) 0.0260(11) Uani 1 1 d . . . . .
C38 C 0.1039(6) 0.8635(5) 0.3233(3) 0.0273(11) Uani 1 1 d . . . . .
H38 H 0.084962 0.802364 0.355449 0.033 Uiso 1 1 calc R . . . .
C28 C 0.4658(6) 0.9715(5) 0.6939(3) 0.0292(12) Uani 1 1 d . . . . .
C12 C 0.3635(5) 0.4110(5) 0.3332(3) 0.0277(11) Uani 1 1 d . . . . .
C11 C 0.4573(5) 0.3950(5) 0.3048(3) 0.0275(11) Uani 1 1 d . . . . .
H11 H 0.468433 0.406985 0.252589 0.033 Uiso 1 1 calc R . . . .
C21 C 0.3010(6) 0.5257(6) 0.9173(4) 0.0328(12) Uani 1 1 d . . . . .
H21 H 0.277225 0.461281 0.946990 0.039 Uiso 1 1 calc R . . . .
C32 C 0.4196(5) 1.0373(5) 0.5711(3) 0.0259(11) Uani 1 1 d . . . . .
C4 C 0.3523(6) 0.2897(5) 0.6746(3) 0.0297(12) Uani 1 1 d . . . . .
C25 C 0.2673(5) 0.5949(5) 0.8000(3) 0.0256(11) Uani 1 1 d . . . . .
H25 H 0.220420 0.579723 0.747581 0.031 Uiso 1 1 calc R . . . .
C17 C 0.1773(6) 0.5475(5) 0.1960(4) 0.0308(12) Uani 1 1 d . . . . .
C31 C 0.5415(6) 1.1401(5) 0.5915(3) 0.0278(11) Uani 1 1 d . . . . .
H31 H 0.567953 1.197286 0.556569 0.033 Uiso 1 1 calc R . . . .
C33 C 0.3827(6) 0.9524(5) 0.6221(3) 0.0286(11) Uani 1 1 d . . . . .
H33 H 0.301172 0.881609 0.608090 0.034 Uiso 1 1 calc R . . . .
C13 C 0.3433(6) 0.3880(5) 0.4083(3) 0.0284(11) Uani 1 1 d . . . . .
H13 H 0.278506 0.397105 0.427049 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5166(6) 0.3423(5) 0.4289(3) 0.0282(11) Uani 1 1 d . . . . .
H9 H 0.572010 0.322873 0.462125 0.034 Uiso 1 1 calc R . . . .
C39 C 0.2701(6) 1.0038(5) 0.4348(3) 0.0292(11) Uani 1 1 d . . . . .
C37 C 0.1991(6) 0.9802(5) 0.3558(3) 0.0277(11) Uani 1 1 d . . . . .
C1 C 0.2883(6) 0.2562(6) 0.8191(3) 0.0310(12) Uani 1 1 d . . . . .
H1 H 0.265838 0.244478 0.868991 0.037 Uiso 1 1 calc R . . . .
C34 C 0.0632(6) 0.9207(6) 0.2025(4) 0.0321(12) Uani 1 1 d . . . . .
H34 H 0.017332 0.900593 0.149374 0.038 Uiso 1 1 calc R . . . .
C30 C 0.6233(5) 1.1583(5) 0.6624(3) 0.0278(11) Uani 1 1 d . . . . .
H30 H 0.705837 1.227812 0.675710 0.033 Uiso 1 1 calc R . . . .
C40 C 0.3355(6) 1.0180(5) 0.4969(3) 0.0289(11) Uani 1 1 d . . . . .
C29 C 0.5856(5) 1.0760(5) 0.7138(3) 0.0277(11) Uani 1 1 d . . . . .
H29 H 0.641308 1.090384 0.762938 0.033 Uiso 1 1 calc R . . . .
C24 C 0.3680(6) 0.7127(5) 0.8324(3) 0.0289(11) Uani 1 1 d . . . . .
C14 C 0.0578(6) 0.6404(6) 0.0994(4) 0.0327(12) Uani 1 1 d . . . . .
H14 H 0.015465 0.672033 0.065838 0.039 Uiso 1 1 calc R . . . .
C10 C 0.5325(6) 0.3621(5) 0.3526(3) 0.0282(11) Uani 1 1 d . . . . .
H10 H 0.596744 0.352556 0.333332 0.034 Uiso 1 1 calc R . . . .
C2 C 0.3802(7) 0.2299(7) 0.8011(4) 0.0402(15) Uani 1 1 d . . . . .
H2 H 0.419623 0.199326 0.837817 0.048 Uiso 1 1 calc R . . . .
C6 C 0.3800(6) 0.3089(5) 0.5981(3) 0.0290(11) Uani 1 1 d . . . . .
C7 C 0.3979(6) 0.3281(5) 0.5335(3) 0.0298(12) Uani 1 1 d . . . . .
C36 C 0.2250(6) 1.0705(5) 0.3088(4) 0.0317(12) Uani 1 1 d . . . . .
H36 H 0.289030 1.151402 0.329266 0.038 Uiso 1 1 calc R . . . .
C19 C 0.2392(6) 0.4992(6) 0.2475(4) 0.0320(12) Uani 1 1 d . . . . .
C20 C 0.2936(6) 0.4573(5) 0.2865(3) 0.0289(11) Uani 1 1 d . . . . .
C35 C 0.1557(6) 1.0399(5) 0.2318(4) 0.0345(13) Uani 1 1 d . . . . .
H35 H 0.171275 1.100005 0.199120 0.041 Uiso 1 1 calc R . . . .
C23 C 0.4340(6) 0.7328(6) 0.9098(4) 0.0366(13) Uani 1 1 d . . . . .
H23 H 0.501880 0.810862 0.933342 0.044 Uiso 1 1 calc R . . . .
N6 N 0.1153(7) 0.6947(7) 0.8938(4) 0.0540(16) Uani 1 1 d . . . . .
C27 C 0.4288(6) 0.8834(5) 0.7453(4) 0.0296(12) Uani 1 1 d . . . . .
C15 C 0.1436(7) 0.6132(6) 0.0722(4) 0.0366(14) Uani 1 1 d . . . . .
H15 H 0.159997 0.625992 0.021006 0.044 Uiso 1 1 calc R . . . .
C22 C 0.3997(6) 0.6380(6) 0.9522(4) 0.0361(13) Uani 1 1 d . . . . .
H22 H 0.444108 0.650471 1.005011 0.043 Uiso 1 1 calc R . . . .
N7 N 0.0951(8) 1.0163(7) 0.6620(5) 0.067(2) Uani 1 1 d . . . . .
C16 C 0.2054(6) 0.5667(6) 0.1213(4) 0.0365(13) Uani 1 1 d . . . . .
H16 H 0.265816 0.548119 0.104503 0.044 Uiso 1 1 calc R . . . .
C26 C 0.3999(6) 0.8067(5) 0.7854(4) 0.0309(12) Uani 1 1 d . . . . .
C3 C 0.4143(6) 0.2488(6) 0.7287(4) 0.0357(14) Uani 1 1 d . . . . .
H3 H 0.479415 0.233978 0.716047 0.043 Uiso 1 1 calc R . . . .
C43 C 0.0967(9) 0.7496(8) 0.8516(5) 0.0536(19) Uani 1 1 d . . . . .
C41 C 0.6219(10) 1.0866(8) 0.9388(5) 0.062(2) Uani 1 1 d . . . . .
C45 C 0.0517(9) 0.9487(8) 0.6104(6) 0.056(2) Uani 1 1 d . . . . .
N5 N 0.5422(11) 1.1127(10) 0.9222(5) 0.087(3) Uani 1 1 d . . . . .
C46 C -0.0081(10) 0.8564(8) 0.5395(6) 0.067(2) Uani 1 1 d . . . . .
H46A H 0.052931 0.873681 0.504995 0.101 Uiso 1 1 calc GR . . . .
H46B H -0.084370 0.856894 0.511381 0.101 Uiso 1 1 calc GR . . . .
H46C H -0.032752 0.777077 0.554825 0.101 Uiso 1 1 calc GR . . . .
C44 C 0.0711(12) 0.8202(10) 0.7953(6) 0.081(3) Uani 1 1 d . . . . .
H44A H -0.014338 0.770364 0.761502 0.121 Uiso 1 1 calc GR . . . .
H44B H 0.135399 0.846405 0.762629 0.121 Uiso 1 1 calc GR . . . .
H44C H 0.075281 0.890847 0.824125 0.121 Uiso 1 1 calc GR . . . .
C42 C 0.7197(10) 1.0515(9) 0.9577(8) 0.080(3) Uani 1 1 d . . . . .
H42A H 0.704796 0.987675 0.916244 0.120 Uiso 1 1 calc GR . . . .
H42B H 0.715799 1.021936 1.008326 0.120 Uiso 1 1 calc GR . . . .
H42C H 0.804421 1.121371 0.961152 0.120 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -7 3 0.0317
0 7 -3 0.0228
-4 8 -4 0.0450
-5 -3 1 0.0503
6 1 0 0.0571
6 -7 4 0.0620
-1 0 11 0.0164
1 0 -11 0.0164
5 -6 -7 0.0410
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
Cl2 Re1 Cl2 180.0 2_566 . ?
Cl2 Re1 Cl1 90.47(6) . 2_566 ?
Cl2 Re1 Cl1 90.47(6) 2_566 . ?
Cl2 Re1 Cl1 89.53(6) . . ?
Cl2 Re1 Cl1 89.53(6) 2_566 2_566 ?
Cl2 Re1 Cl3 91.06(7) . 2_566 ?
Cl2 Re1 Cl3 91.06(7) 2_566 . ?
Cl2 Re1 Cl3 88.94(7) 2_566 2_566 ?
Cl2 Re1 Cl3 88.94(7) . . ?
Cl1 Re1 Cl1 180.00(9) . 2_566 ?
Cl1 Re1 Cl3 90.11(7) . 2_566 ?
Cl1 Re1 Cl3 89.89(7) . . ?
Cl1 Re1 Cl3 89.89(7) 2_566 2_566 ?
Cl1 Re1 Cl3 90.11(7) 2_566 . ?
Cl3 Re1 Cl3 180.0 2_566 . ?
N4 Pd1 N3 178.21(18) 2_566 . ?
N4 Pd1 N1 89.21(19) 2_566 . ?
N4 Pd1 N2 91.57(19) 2_566 2_566 ?
N3 Pd1 N1 89.52(19) . . ?
N3 Pd1 N2 89.67(19) . 2_566 ?
N1 Pd1 N2 178.65(18) . 2_566 ?
F5 P1 F6 177.9(3) . . ?
F1 P1 F6 89.6(3) . . ?
F1 P1 F5 89.0(3) . . ?
F3 P1 F6 91.1(3) . . ?
F3 P1 F5 90.4(3) . . ?
F3 P1 F1 178.8(4) . . ?
F3 P1 F4 93.4(4) . . ?
F3 P1 F2 90.5(4) . . ?
F4 P1 F6 90.0(2) . . ?
F4 P1 F5 88.4(3) . . ?
F4 P1 F1 87.6(4) . . ?
F2 P1 F6 90.8(3) . . ?
F2 P1 F5 90.7(3) . . ?
F2 P1 F1 88.5(4) . . ?
F2 P1 F4 176.0(4) . . ?
C38 N4 Pd1 121.2(4) . 2_566 ?
C34 N4 Pd1 120.6(4) . 2_566 ?
C34 N4 C38 118.1(5) . . ?
C21 N3 Pd1 118.5(4) . . ?
C25 N3 Pd1 121.8(4) . . ?
C25 N3 C21 119.8(5) . . ?
C5 N1 Pd1 120.4(4) . . ?
C5 N1 C1 119.6(5) . . ?
C1 N1 Pd1 120.0(4) . . ?
C18 N2 Pd1 121.9(4) . 2_566 ?
C18 N2 C14 119.0(5) . . ?
C14 N2 Pd1 119.0(4) . 2_566 ?
N1 C5 H5 118.9 . . ?
N1 C5 C4 122.3(5) . . ?
C4 C5 H5 118.9 . . ?
N2 C18 H18 119.1 . . ?
N2 C18 C17 121.9(5) . . ?
C17 C18 H18 119.1 . . ?
C13 C8 C7 119.8(5) . . ?
C9 C8 C13 119.2(5) . . ?
C9 C8 C7 121.0(5) . . ?
N4 C38 H38 118.6 . . ?
N4 C38 C37 122.9(5) . . ?
C37 C38 H38 118.6 . . ?
C33 C28 C27 120.0(6) . . ?
C29 C28 C33 119.4(5) . . ?
C29 C28 C27 120.5(5) . . ?
C11 C12 C20 119.8(5) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 C20 120.1(5) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 C12 119.7(5) . . ?
C10 C11 H11 120.2 . . ?
N3 C21 H21 119.1 . . ?
N3 C21 C22 121.9(6) . . ?
C22 C21 H21 119.1 . . ?
C31 C32 C40 120.1(5) . . ?
C33 C32 C31 119.4(5) . . ?
C33 C32 C40 120.5(5) . . ?
C5 C4 C6 119.2(5) . . ?
C3 C4 C5 118.0(5) . . ?
C3 C4 C6 122.9(5) . . ?
N3 C25 H25 119.4 . . ?
N3 C25 C24 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C18 C17 C19 121.3(6) . . ?
C18 C17 C16 118.8(5) . . ?
C16 C17 C19 120.0(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 C32 120.2(5) . . ?
C30 C31 H31 119.9 . . ?
C28 C33 H33 120.0 . . ?
C32 C33 C28 120.1(5) . . ?
C32 C33 H33 120.0 . . ?
C8 C13 H13 120.0 . . ?
C12 C13 C8 120.0(5) . . ?
C12 C13 H13 120.0 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.8(5) . . ?
C10 C9 H9 120.1 . . ?
C40 C39 C37 173.0(6) . . ?
C38 C37 C39 119.4(5) . . ?
C38 C37 C36 118.4(5) . . ?
C36 C37 C39 122.1(6) . . ?
N1 C1 H1 119.3 . . ?
N1 C1 C2 121.5(5) . . ?
C2 C1 H1 119.3 . . ?
N4 C34 H34 119.0 . . ?
N4 C34 C35 121.9(6) . . ?
C35 C34 H34 119.0 . . ?
C31 C30 H30 119.8 . . ?
C29 C30 C31 120.4(5) . . ?
C29 C30 H30 119.8 . . ?
C39 C40 C32 177.7(7) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29 119.8 . . ?
C25 C24 C26 119.8(5) . . ?
C23 C24 C25 118.2(5) . . ?
C23 C24 C26 122.0(6) . . ?
N2 C14 H14 118.6 . . ?
N2 C14 C15 122.7(5) . . ?
C15 C14 H14 118.6 . . ?
C11 C10 C9 121.2(5) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 119.1(5) . . ?
C3 C2 H2 120.5 . . ?
C7 C6 C4 175.7(6) . . ?
C6 C7 C8 179.7(6) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 C37 118.8(6) . . ?
C35 C36 H36 120.6 . . ?
C20 C19 C17 176.0(7) . . ?
C19 C20 C12 177.8(7) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.8(6) . . ?
C36 C35 H35 120.1 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.4(6) . . ?
C22 C23 H23 120.3 . . ?
C26 C27 C28 176.4(6) . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.6(6) . . ?
C16 C15 H15 120.7 . . ?
C21 C22 C23 119.5(6) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 H16 120.5 . . ?
C27 C26 C24 177.8(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 C4 119.6(5) . . ?
C2 C3 H3 120.2 . . ?
N6 C43 C44 179.2(11) . . ?
N5 C41 C42 178.5(11) . . ?
N7 C45 C46 179.7(12) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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
Re1 Cl2 2.3522(15) 2_566 ?
Re1 Cl2 2.3522(15) . ?
Re1 Cl1 2.3610(16) . ?
Re1 Cl1 2.3610(16) 2_566 ?
Re1 Cl3 2.3635(17) 2_566 ?
Re1 Cl3 2.3635(17) . ?
Pd1 N4 1.994(5) 2_566 ?
Pd1 N3 2.000(5) . ?
Pd1 N1 2.004(5) . ?
Pd1 N2 2.013(5) 2_566 ?
P1 F6 1.616(4) . ?
P1 F5 1.607(4) . ?
P1 F1 1.595(5) . ?
P1 F3 1.548(5) . ?
P1 F4 1.582(5) . ?
P1 F2 1.564(5) . ?
N4 C38 1.360(7) . ?
N4 C34 1.350(7) . ?
N3 C21 1.350(8) . ?
N3 C25 1.342(7) . ?
N1 C5 1.331(7) . ?
N1 C1 1.353(7) . ?
N2 C18 1.340(7) . ?
N2 C14 1.349(7) . ?
C5 H5 0.9500 . ?
C5 C4 1.397(8) . ?
C18 H18 0.9500 . ?
C18 C17 1.394(8) . ?
C8 C13 1.409(8) . ?
C8 C9 1.397(8) . ?
C8 C7 1.426(8) . ?
C38 H38 0.9500 . ?
C38 C37 1.389(8) . ?
C28 C33 1.402(8) . ?
C28 C29 1.399(9) . ?
C28 C27 1.430(8) . ?
C12 C11 1.403(8) . ?
C12 C13 1.390(8) . ?
C12 C20 1.433(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.369(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.375(9) . ?
C32 C31 1.404(8) . ?
C32 C33 1.398(8) . ?
C32 C40 1.439(8) . ?
C4 C6 1.431(8) . ?
C4 C3 1.391(8) . ?
C25 H25 0.9500 . ?
C25 C24 1.416(8) . ?
C17 C19 1.431(8) . ?
C17 C16 1.403(9) . ?
C31 H31 0.9500 . ?
C31 C30 1.385(8) . ?
C33 H33 0.9500 . ?
C13 H13 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.394(8) . ?
C39 C37 1.432(8) . ?
C39 C40 1.183(9) . ?
C37 C36 1.399(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.391(9) . ?
C30 H30 0.9500 . ?
C30 C29 1.382(8) . ?
C29 H29 0.9500 . ?
C24 C23 1.394(9) . ?
C24 C26 1.430(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(8) . ?
C10 H10 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.387(9) . ?
C6 C7 1.196(8) . ?
C36 H36 0.9500 . ?
C36 C35 1.385(9) . ?
C19 C20 1.193(8) . ?
C35 H35 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.385(9) . ?
N6 C43 1.117(11) . ?
C27 C26 1.187(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(8) . ?
C22 H22 0.9500 . ?
N7 C45 1.072(12) . ?
C16 H16 0.9500 . ?
C3 H3 0.9500 . ?
C43 C44 1.467(12) . ?
C41 N5 1.169(13) . ?
C41 C42 1.456(13) . ?
C45 C46 1.468(13) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 Cl2 0.95 2.61 3.540(6) 166.9 .
C38 H38 Cl1 0.95 2.89 3.752(6) 151.9 2_566
C21 H21 F6 0.95 2.54 3.416(8) 153.5 2_667
C21 H21 F1 0.95 2.29 3.155(8) 150.5 2_667
C25 H25 Cl3 0.95 2.96 3.829(6) 152.3 .
C1 H1 F6 0.95 2.57 3.439(7) 151.7 2_667
C1 H1 F4 0.95 2.30 3.173(8) 153.3 2_667
C34 H34 F6 0.95 2.50 3.364(8) 152.1 1_454
C14 H14 F6 0.95 2.47 3.357(7) 154.9 1_454
C2 H2 N5 0.95 2.58 3.527(10) 171.9 1_545
C35 H35 F5 0.95 2.38 3.224(7) 148.5 2_676
C15 H15 N6 0.95 2.51 3.354(9) 148.5 1_554
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
Pd1 N4 C38 C37 179.6(4) 2_566 . . . ?
Pd1 N4 C34 C35 179.3(5) 2_566 . . . ?
Pd1 N3 C21 C22 178.3(5) . . . . ?
Pd1 N3 C25 C24 -178.3(4) . . . . ?
Pd1 N1 C5 C4 179.5(4) . . . . ?
Pd1 N1 C1 C2 -179.4(5) . . . . ?
Pd1 N2 C18 C17 178.9(4) 2_566 . . . ?
Pd1 N2 C14 C15 -178.7(5) 2_566 . . . ?
N4 C38 C37 C39 -176.7(5) . . . . ?
N4 C38 C37 C36 1.3(8) . . . . ?
N4 C34 C35 C36 1.1(10) . . . . ?
N3 C21 C22 C23 0.8(10) . . . . ?
N3 C25 C24 C23 -0.8(8) . . . . ?
N3 C25 C24 C26 178.6(5) . . . . ?
N1 C5 C4 C6 179.7(6) . . . . ?
N1 C5 C4 C3 -1.2(9) . . . . ?
N1 C1 C2 C3 1.0(11) . . . . ?
N2 C18 C17 C19 179.1(6) . . . . ?
N2 C18 C17 C16 -0.6(9) . . . . ?
N2 C14 C15 C16 0.1(11) . . . . ?
C5 N1 C1 C2 0.2(10) . . . . ?
C5 C4 C3 C2 2.3(10) . . . . ?
C18 N2 C14 C15 -1.3(9) . . . . ?
C18 C17 C16 C15 -0.6(10) . . . . ?
C8 C9 C10 C11 2.7(9) . . . . ?
C38 N4 C34 C35 -0.3(9) . . . . ?
C38 C37 C36 C35 -0.5(9) . . . . ?
C12 C11 C10 C9 1.0(9) . . . . ?
C11 C12 C13 C8 1.4(9) . . . . ?
C21 N3 C25 C24 1.5(8) . . . . ?
C32 C31 C30 C29 -0.3(8) . . . . ?
C25 N3 C21 C22 -1.5(9) . . . . ?
C25 C24 C23 C22 0.2(9) . . . . ?
C31 C32 C33 C28 1.6(8) . . . . ?
C31 C30 C29 C28 1.9(8) . . . . ?
C33 C28 C29 C30 -1.7(8) . . . . ?
C33 C32 C31 C30 -1.4(8) . . . . ?
C13 C8 C9 C10 -4.3(9) . . . . ?
C13 C12 C11 C10 -3.0(9) . . . . ?
C9 C8 C13 C12 2.3(9) . . . . ?
C39 C37 C36 C35 177.4(6) . . . . ?
C37 C36 C35 C34 -0.6(9) . . . . ?
C1 N1 C5 C4 0.0(9) . . . . ?
C1 C2 C3 C4 -2.2(11) . . . . ?
C34 N4 C38 C37 -0.9(8) . . . . ?
C40 C32 C31 C30 -179.2(5) . . . . ?
C40 C32 C33 C28 179.4(5) . . . . ?
C29 C28 C33 C32 -0.1(8) . . . . ?
C24 C23 C22 C21 -0.2(10) . . . . ?
C14 N2 C18 C17 1.5(9) . . . . ?
C14 C15 C16 C17 0.9(11) . . . . ?
C6 C4 C3 C2 -178.6(7) . . . . ?
C7 C8 C13 C12 179.7(6) . . . . ?
C7 C8 C9 C10 178.3(6) . . . . ?
C19 C17 C16 C15 179.7(6) . . . . ?
C20 C12 C11 C10 173.6(6) . . . . ?
C20 C12 C13 C8 -175.3(5) . . . . ?
C27 C28 C33 C32 -178.9(5) . . . . ?
C27 C28 C29 C30 177.1(5) . . . . ?
C26 C24 C23 C22 -179.3(6) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0003 -6.9910 3.0098 -0.1053 0.3434 0.8954
0.0003 6.9910 -3.0098 0.1053 -0.3434 -0.8954
-4.0007 7.9899 -3.9922 0.2463 -0.7892 -0.5871
-5.0012 -2.9960 1.0277 0.0737 -0.3448 0.9281
6.0014 0.9985 -0.0297 -0.1352 0.5421 -0.7813
6.0014 -6.9913 3.9813 -0.3072 0.9399 0.2407
-0.9928 -0.0013 11.0009 -0.9752 0.0055 0.0837
0.9928 0.0013 -11.0009 0.9752 -0.0055 -0.0837
4.9942 -5.9912 -7.0117 0.6815 0.6937 0.2456
