A ferrocene-templated Pd-bearing molecular reactor.
Kasprzak, Artur; Guńka, Piotr A; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6974–6979; doi:10.1039/d0dt01366h

data_7704395
_publ_section_title
;
 A ferrocene-templated Pd-bearing molecular reactor.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6974
_journal_page_last               6979
_journal_paper_doi               10.1039/d0dt01366h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C84 H60 Fe3 N6'
_chemical_formula_sum            'C84 H60 Fe3 N6'
_chemical_formula_weight         1320.93
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-05 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.9627(11)
_cell_length_b                   24.9627(11)
_cell_length_c                   20.5795(11)
_cell_measurement_reflns_used    2783
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.8120
_cell_measurement_theta_min      3.3760
_cell_volume                     11105.8(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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    -43.00  10.00   0.50  100.00    --   15.71 -38.00  90.00  106
  2  \w    -42.00  32.00   0.50  100.00    --   15.71 -38.00-150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0194972000
_diffrn_orient_matrix_UB_12      -0.0207269000
_diffrn_orient_matrix_UB_13      -0.0243091000
_diffrn_orient_matrix_UB_21      -0.0189633000
_diffrn_orient_matrix_UB_22      -0.0209585000
_diffrn_orient_matrix_UB_23      0.0244287000
_diffrn_orient_matrix_UB_31      -0.0183514000
_diffrn_orient_matrix_UB_32      0.0143840000
_diffrn_orient_matrix_UB_33      0.0005773000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11433
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, benzene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3409
_reflns_number_total             5389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01366h1.cif
_cod_data_source_block           md611_ak01_sq
_cod_depositor_comments          'Adding full bibliography for 7704395.cif.'
_cod_original_cell_volume        11105.8(11)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7704395
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C84H60Fe3N6
_chemical_oxdiff_usercomment     'crystallized from benzene solution'
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.859
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C32(H32), C31(H31), C14(H14), C11(H11), C6(H6), C12(H12), C25(H25),
 C5(H5), C26(H26), C22(H22), C29(H29), C2(H2), C28(H28), C4(H4), C24(H24),
 C9(H9), C23(H23), C3(H3), C8(H8)
;
_shelx_res_checksum              39377
_shelx_hkl_checksum              1422
_shelx_fab_checksum              40446
_olex2_date_sample_data_collection 2019-11-27
_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 1.065
_oxdiff_exptl_absorpt_empirical_full_min 0.965