Influence of Solvent in Crystal Engineering: A Significant Change to the Order-Disorder Transition in Ferrocene.
Bear, Joseph C.; Cockcroft, Jeremy K.; Williams, Jeffrey H.; Journal of the American Chemical Society 142 (2020) 1731–1734; doi:10.1021/jacs.9b11895

data_4133968
_publ_section_title
;
 Influence of Solvent in Crystal Engineering: A Significant Change to the
 Order-Disorder Transition in Ferrocene.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1731
_journal_page_last               1734
_journal_paper_doi               10.1021/jacs.9b11895
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C10 H10 Fe, 2(C3 F3)'
_chemical_formula_sum            'C16 H10 F6 Fe'
_chemical_formula_weight         372.09
_chemical_name_systematic        Ferrocene:hexafluorobenzene
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                78.035(5)
_cell_angle_beta                 76.862(6)
_cell_angle_gamma                84.337(5)
_cell_formula_units_Z            2
_cell_length_a                   7.1724(5)
_cell_length_b                   9.0455(5)
_cell_length_c                   11.3389(7)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9880
_cell_measurement_theta_min      3.5990
_cell_volume                     699.80(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_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    -67.00 -38.00   1.00    2.00    --   -9.99 126.00  59.75   29
  2  \w    -10.00  56.00   1.00    2.00    --   11.17  77.00-150.00   66
  3  \w     -2.00  87.00   1.00    2.00    --   11.17  77.00  90.00   89
  4  \w    -16.00  84.00   1.00    2.00    --   11.17  57.00   0.00  100
  5  \w    -63.00  43.00   1.00    2.00    --   11.17 -72.00  31.65  106
  6  \w    -19.00  52.00   1.00    2.00    --   11.17 -99.00 -60.00   71
  7  \w    -71.00 -34.00   1.00    2.00    --   11.17   0.00  60.00   37
  8  \w     46.00  99.00   1.00    2.00    --   11.17   0.00  60.00   53
  9  \w     18.00  88.00   1.00    2.00    --   11.17-155.00-128.36   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0070529000
_diffrn_orient_matrix_UB_12      0.0786876000
_diffrn_orient_matrix_UB_13      -0.0237365000
_diffrn_orient_matrix_UB_21      -0.0787688000
_diffrn_orient_matrix_UB_22      -0.0002321000
_diffrn_orient_matrix_UB_23      -0.0281056000
_diffrn_orient_matrix_UB_31      -0.0639413000
_diffrn_orient_matrix_UB_32      0.0158742000
_diffrn_orient_matrix_UB_33      0.0541182000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11866
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_preparation       'Ferrocene dissolved in hot C6F6'
_exptl_crystal_recrystallization_method
'Crystals grown using C6F6 as soilvent in an NMR tube stood in hot water'
_exptl_crystal_size_max          0.722
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0381
_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/[\s^2^(Fo^2^)+(0.0426P)^2^+0.1062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2787
_reflns_number_total             3334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11895_si_002.cif
_cod_data_source_block           exp_1368
_cod_depositor_comments
'Adding full bibliography for 4133967--4133980.cif.'
_cod_database_code               4133968
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe C16 F6 H10'
_chemical_oxdiff_usercomment     'Same crystal as used 13 Dec in capillary'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.493
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              19670
_shelx_hkl_checksum              4099
_olex2_date_sample_data_collection 2018-12-21
_olex2_exptl_crystal_mounting_method 'Inside 0.5mm X-ray capillary'
_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 39.749
_oxdiff_exptl_absorpt_empirical_full_min 0.440