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_4133967
_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     direct
_audit_creation_date             2019-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                78.169(4)
_cell_angle_beta                 76.779(5)
_cell_angle_gamma                84.426(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1737(4)
_cell_length_b                   9.0077(5)
_cell_length_c                   11.2753(6)
_cell_measurement_reflns_used    7167
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.2780
_cell_measurement_theta_min      4.4650
_cell_volume                     693.25(7)
_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      C6F6
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.962
_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    -11.00  64.00   1.00    1.00    --  -10.23  38.00  60.00   75
  2  \w      0.00  83.00   1.00    1.00    --   11.09  57.00  60.00   83
  3  \w    -16.00  84.00   1.00    1.00    --   11.09  77.00 -60.00  100
  4  \w    -17.00  84.00   1.00    1.00    --   11.09  57.00-180.00  101
  5  \w     -6.00  62.00   1.00    1.00    --   11.09-116.00  13.32   68
  6  \w    -20.00  52.00   1.00    1.00    --   11.09 -99.00 150.00   72
  7  \w    -48.00  44.00   1.00    1.00    --   11.09 -77.00-120.00   92
  8  \w    -68.00 -43.00   1.00    1.00    --  -10.23 127.00 -21.71   25
;
_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      -0.0718161000
_diffrn_orient_matrix_UB_12      -0.0346640000
_diffrn_orient_matrix_UB_13      -0.0172940000
_diffrn_orient_matrix_UB_21      -0.0658002000
_diffrn_orient_matrix_UB_22      0.0125184000
_diffrn_orient_matrix_UB_23      0.0548811000
_diffrn_orient_matrix_UB_31      -0.0292825000
_diffrn_orient_matrix_UB_32      0.0716410000
_diffrn_orient_matrix_UB_33      -0.0319201000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11766
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.273
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.170
_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    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_preparation       'Ferrocene disssolved in hot C6F6'
_exptl_crystal_recrystallization_method
'Crystals grown using C6F6 as solvent in an NMR tube stood in hot water'
_exptl_crystal_size_max          0.778
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.322
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0289P)^2^+0.2676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2941
_reflns_number_total             3304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11895_si_002.cif
_cod_data_source_block           exp_1219
_cod_depositor_comments
'Adding full bibliography for 4133967--4133980.cif.'
_cod_database_code               4133967
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe1 C16 F6 H10'
_chemical_oxdiff_usercomment     'In sealed capillary'
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.490
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              41285
_shelx_hkl_checksum              6449
_olex2_date_sample_data_collection 2018-10-25
_olex2_exptl_crystal_mounting_method
'Crystal sealed in 1 mm X-ray glass capillary with excess solvent removed'
_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 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.857