Guest-induced magnetic exchange in paramagnetic [M2L4]4+ coordination cages
Singh, Mukesh K.; Etcheverry-Berríos, Alvaro; Vallejo, Julia; Sanz, Sergio; Martínez-Lillo, José; Nichol, Gary S.; Lusby, Paul J.; Brechin, Euan K.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01385A

data_7710293
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00  29.00   1.00   10.00    --  -41.42  57.00-150.00   97
  2  \w   -127.00 -34.00   1.00   10.00    --  -41.42 178.00-180.00   93
  3  \w   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00  60.00   97
  4  \w     19.00 114.00   1.00   10.00    --   41.42  38.00   0.00   95
  5  \w      1.00  81.00   1.00   10.00    --   41.42 -99.00   0.00   80
  6  \w     87.00 178.00   1.00   30.00    --  111.00  45.00  60.00   91
  7  \w     40.00 125.00   1.00   30.00    --  111.00-131.00 138.00   85
  8  \w     41.00 128.00   1.00   30.00    --  111.00-138.00 -36.00   87
  9  \w     80.00 178.00   1.00   30.00    --  111.00  77.00   0.00   98
 10  \w     94.00 178.00   1.00   30.00    --  111.00 125.00-120.00   84
 11  \w     83.00 178.00   1.00   30.00    --  111.00  61.00 120.00   95
 12  \w     87.00 178.00   1.00   30.00    --  111.00  30.00 -30.00   91
 13  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00-150.00   79
 14  \w     39.00 121.00   1.00   30.00    --  111.00-125.00   0.00   82
 15  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00 150.00   79
 16  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00 -30.00   79
 17  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00 -30.00   98
 18  \w     36.00 135.00   1.00   30.00    --  111.00 -30.00  90.00   99
 19  \w   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00 150.00   97
 20  \w   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00 -30.00  105
 21  \w   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00-150.00   97
 22  \w   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00  60.00  105
 23  \w   -112.00 -65.00   1.00   10.00    --  -41.42-138.00 -36.00   47
 24  \w     87.00 178.00   1.00   30.00    --  111.00  30.00 -90.00   91
 25  \w     87.00 178.00   1.00   30.00    --  111.00  30.00-150.00   91
 26  \w     83.00 178.00   1.00   30.00    --  111.00  61.00-150.00   95
 27  \w     83.00 178.00   1.00   30.00    --  111.00  61.00  90.00   95
 28  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0830P)^2^+4.3337P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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'
_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)
;
_shelx_res_checksum              44238
_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