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_4133978
_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         '0.5(C20 H20 Fe2), C6 F6'
_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           '-B 1'
_space_group_name_H-M_alt        'B -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                76.583(6)
_cell_angle_beta                 77.727(6)
_cell_angle_gamma                83.757(5)
_cell_formula_units_Z            2
_cell_length_a                   7.1618(5)
_cell_length_b                   9.2536(6)
_cell_length_c                   11.8972(9)
_cell_measurement_reflns_used    2922
_cell_measurement_temperature    302.5
_cell_measurement_theta_max      26.4240
_cell_measurement_theta_min      5.1370
_cell_volume                     747.94(9)
_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      302.5
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_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    -11.00  87.00   1.00    2.00    --   11.17  77.00  90.00   98
  2  \w     13.00  77.00   1.00    2.00    --   11.17  38.00-150.00   64
  3  \w    -53.00  39.00   1.00    2.00    --   11.17 -57.00-180.00   92
  4  \w     -2.00  58.00   1.00    2.00    --   11.17-110.00 120.00   60
  5  \w    -17.00  52.00   1.00    2.00    --   11.17 -99.00 -60.00   69
  6  \w     -7.00  67.00   1.00    2.00    --   11.17  38.00 -60.00   74
  7  \w      4.00  52.00   1.00    2.00    --   11.17 -99.00   0.00   48
  8  \w     27.00  84.00   1.00    2.00    --   11.17  57.00 -30.00   57
;
_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      0.0215465000
_diffrn_orient_matrix_UB_12      -0.0756139000
_diffrn_orient_matrix_UB_13      0.0254445000
_diffrn_orient_matrix_UB_21      -0.0297711000
_diffrn_orient_matrix_UB_22      0.0153703000
_diffrn_orient_matrix_UB_23      0.0570534000
_diffrn_orient_matrix_UB_31      -0.0946715000
_diffrn_orient_matrix_UB_32      -0.0167470000
_diffrn_orient_matrix_UB_33      0.0008339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4853
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.251
_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    1.652
_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 solvent 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         0.280
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1271
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.374
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0522P)^2^+0.4173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1240
_reflns_number_total             1271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11895_si_002.cif
_cod_data_source_block           exp_1341
_cod_depositor_comments
'Adding full bibliography for 4133967--4133980.cif.'
_cod_original_sg_number          -1
_cod_original_sg_symbol_H-M      '-B 1'
_cod_database_code               4133978
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe C16 H10 F6'
_chemical_oxdiff_usercomment     'In capillary'
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.513
_reflns_odcompleteness_completeness 49.77
_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. Restrained distances
 C7-C9A \\sim C7-C10A \\sim C8-C10A \\sim C8-C11A \\sim C9-C11A \\sim C9-C7A
\\sim C10-C7A \\sim C10-C8A ~
 C11-C8A \\sim C11-C9A
 with sigma of 0.02
 C7-C7A \\sim C8-C8A \\sim C9-C9A \\sim C10-C10A \\sim C11-C11A
 with sigma of 0.02
 Fe1-C7 \\sim Fe1-C7A \\sim Fe1-C8 \\sim Fe1-C8A \\sim Fe1-C9 \\sim Fe1-C9A
\\sim Fe1-C10 \\sim Fe1-C10A ~
 Fe1-C11 \\sim Fe1-C11A
 with sigma of 0.02
3. Rigid bond restraints
 Fe1, C7, Fe1, C8, Fe1, C9, Fe1, C10, Fe1, C11, Fe1, C7A, Fe1, C8A, Fe1, C9A,
 Fe1, C10A, Fe1, C11A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C7, C9A, C7, C10A, C8, C10A, C8, C11A, C9, C11A, C9, C7A, C10, C7A, C10, C8A,
 C11, C8A, C11, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5)
 C11(0.5) H11(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5)
 C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C7A(H7A), C8A(H8A), C9A(H9A),
 C10A(H10A), C11A(H11A)
;
_shelx_res_checksum              77261
_shelx_hkl_checksum              99272
_olex2_date_sample_data_collection 2018-12-13
_olex2_exptl_crystal_mounting_method 'Inside 1.0 mm 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 1.848
_oxdiff_exptl_absorpt_empirical_full_min 0.762