Redox Active [Pd2L4]4+ Cages Constructed from Rotationally Flexible 1,1′-Disubstituted Ferrocene Ligands
Vasdev, Roan A. S.; Findlay, James A.; Garden, Anna L.; Crowley, James D.; Chemical Communications  (2019) –; doi:10.1039/C9CC03321A

data_7123583
_publ_section_title
;
 Redox Active [Pd2L4]4+ Cages Constructed from Rotationally Flexible
 1,1&#x2032;-Disubstituted Ferrocene Ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03321A
_journal_year                    2019
_chemical_formula_moiety         'C96 H64 Fe4 N8 Pd2, 4(F6 Sb), C2 H3 N'
_chemical_formula_sum            'C98 H67 F24 Fe4 N9 Pd2 Sb4'
_chemical_formula_weight         2749.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-07 deposited with the CCDC.    2019-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                86.322(2)
_cell_angle_beta                 77.790(3)
_cell_angle_gamma                88.585(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7055(6)
_cell_length_b                   19.5133(7)
_cell_length_c                   25.8602(7)
_cell_measurement_reflns_used    10550
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.1170
_cell_measurement_theta_min      4.1730
_cell_volume                     6253.1(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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   -106.00 -19.00   1.00   10.50    --  -42.04 -38.00 120.00   87
  2  \w   -113.00 -21.00   1.00   10.50    --  -42.04 -57.00   0.00   92
  3  \w    -67.00  32.00   1.00   10.50    --  -42.04  38.00 -60.00   99
  4  \w    -70.00 -25.00   1.00   10.50    --  -42.04  57.00 150.00   45
  5  \w     52.00  89.00   1.00   10.50    --   42.04-109.00 -88.00   37
  6  \w     33.00  81.00   1.00   42.00    --  108.40 -77.00   0.00   48
  7  \w     26.00  60.00   1.00   42.00    --  108.40 -95.00 -30.00   34
  8  \w     84.00 177.00   1.00   42.00    --  108.40  77.00 -30.00   93
  9  \w     63.00 121.00   1.00   42.00    --  108.40-125.00 -90.00   58
 10  \w    128.00 177.00   1.00   42.00    --  108.40  45.00-180.00   49
 11  \w     35.00 105.00   1.00   42.00    --  108.40 -77.00 -90.00   70
 12  \w     86.00 176.00   1.00   42.00    --  108.40  30.00 120.00   90
 13  \w    106.00 157.00   1.00   42.00    --  108.40 109.00   8.00   51
 14  \w     87.00 132.00   1.00   42.00    --  108.40 -77.00   0.00   45
 15  \w     36.00 110.00   1.00   42.00    --  108.40-125.00-180.00   74
 16  \w    127.00 176.00   1.00   42.00    --  108.40  61.00  60.00   49
 17  \w    110.00 162.00   1.00   42.00    --  108.40 125.00 -60.00   52
 18  \w     80.00 109.00   1.00   42.00    --  108.40 -95.00   0.00   29
 19  \w     79.00 122.00   1.00   42.00    --  108.40  61.00  60.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0762652000
_diffrn_orient_matrix_UB_12      -0.0592950000
_diffrn_orient_matrix_UB_13      -0.0024998000
_diffrn_orient_matrix_UB_21      -0.0974097000
_diffrn_orient_matrix_UB_22      0.0492785000
_diffrn_orient_matrix_UB_23      0.0125908000
_diffrn_orient_matrix_UB_31      0.0093508000
_diffrn_orient_matrix_UB_32      0.0177566000
_diffrn_orient_matrix_UB_33      -0.0596982000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43061
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       plate
_exptl_crystal_F_000             2668
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.05
_refine_diff_density_max         9.261
_refine_diff_density_min         -2.294
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         23570
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.1134
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3057
_refine_ls_wR_factor_ref         0.3436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14885
_reflns_number_total             23570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03321a3.cif
_cod_data_source_block           jaf298b
_cod_database_code               7123583
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C96H64F24Fe4N8Pd2Sb4
_chemical_oxdiff_usercomment     L040
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: Sb4A(0.5) Sb4B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C48(H48), C78(H78), C36(H36), C37(H37), C26(H26), C1(H1), C22(H22),
 C54(H54), C74(H74), C73(H73), C72(H72), C25(H25), C23(H23), C11(H11), C61(H61),
  C47(H47), C45(H45), C35(H35), C46(H46), C97(H97), C38(H38), C9(H9), C2(H2),
 C10(H10), C21(H21), C60(H60), C85(H85), C33(H33), C96(H96), C34(H34), C13(H13),
  C50(H50), C14(H14), C40(H40), C12(H12), C84(H84), C16(H16), C95(H95),
 C71(H71), C58(H58), C70(H70), C28(H28), C76(H76), C59(H59), C39(H39), C82(H82),
  C15(H15), C94(H94), C27(H27), C51(H51), C64(H64), C75(H75), C4(H4), C52(H52),
 C83(H83), C65(H65), C62(H62), C87(H87), C63(H63), C89(H89), C3(H3), C86(H86),
 C88(H88)
4.b Idealised Me refined as rotating group:
 C99(H99A,H99B,H99C)
;
_shelx_res_checksum              7899
_shelx_fab_checksum              79608
_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 2.676
_oxdiff_exptl_absorpt_empirical_full_min 0.565