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_4133980
_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 Ru'
_chemical_formula_sum            'C10 H10 Ru'
_chemical_formula_weight         231.25
_chemical_name_systematic        Bis(cyclopentadienyl)ruthenium(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.02290(10)
_cell_length_b                   8.8503(2)
_cell_length_c                   12.7614(2)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.4450
_cell_measurement_theta_min      3.4330
_cell_volume                     793.18(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -56.00 -11.00   1.00    1.00    --  -42.62 -77.00  30.00   45
  2  \w   -118.00 -10.00   1.00    1.00    --  -42.62 -77.00 -30.00  108
  3  \w    -76.00 -19.00   1.00    1.00    --  -42.62 -38.00-150.00   57
  4  \w   -114.00 -10.00   1.00    1.00    --  -42.62 -77.00-150.00  104
  5  \w    -66.00  29.00   1.00    1.00    --  -42.62  38.00 -90.00   95
  6  \w    -63.00  21.00   1.00    1.00    --  -42.62  38.00   0.00   84
  7  \w    -84.00 -10.00   1.00    1.00    --  -42.62 -77.00 120.00   74
  8  \w     23.00  56.00   1.00    1.00    --   42.62-125.00-180.00   33
  9  \w     68.00  98.00   1.00    1.00    --   42.62-125.00-180.00   30
 10  \w     -3.00  71.00   1.00    1.00    --   42.62 -95.00  62.00   74
 11  \w     78.00 177.00   1.00    1.00    --  104.49  61.00 120.00   99
 12  \w     72.00  98.00   1.00    1.00    --  104.49  77.00   0.00   26
 13  \w     73.00  98.00   1.00    1.00    --  104.49  77.00-180.00   25
 14  \w     72.00 109.00   1.00    1.00    --  104.49  77.00 -60.00   37
 15  \w     75.00 107.00   1.00    1.00    --  104.49  61.00-120.00   32
 16  \w    146.00 172.00   1.00    1.00    --  104.49  61.00-180.00   26
 17  \w     75.00 143.00   1.00    1.00    --  104.49  61.00-180.00   68
 18  \w     73.00 176.00   1.00    1.00    --  104.49  77.00-120.00  103
 19  \w     76.00 107.00   1.00    1.00    --  104.49  61.00 -60.00   31
 20  \w     32.00 110.00   1.00    1.00    --  104.49-125.00   0.00   78
 21  \w     79.00 175.00   1.00    1.00    --  104.49  61.00  60.00   96
 22  \w     72.00  98.00   1.00    1.00    --  104.49  77.00 150.00   26
 23  \w     22.00 109.00   1.00    1.00    --  104.49 -94.00-180.00   87
 24  \w     49.00 112.00   1.00    1.00    --  104.49 -61.00-180.00   63
 25  \w     76.00 163.00   1.00    1.00    --  104.49  61.00  30.00   87
 26  \w     76.00 101.00   1.00    1.00    --  104.49  61.00  90.00   25
 27  \w     72.00  98.00   1.00    1.00    --  104.49  77.00  90.00   26
 28  \w     74.00 108.00   1.00    1.00    --  104.49 -94.00  90.00   34
 29  \w     72.00  99.00   1.00    1.00    --  104.49  77.00 -30.00   27
 30  \w     72.00  98.00   1.00    1.00    --  104.49  77.00-150.00   26
 31  \w     44.00  71.00   1.00    1.00    --  104.49 -94.00  90.00   27
 32  \w     23.00 106.00   1.00    1.00    --  104.49 -94.00  30.00   83
 33  \w     72.00  98.00   1.00    1.00    --  104.49  77.00 120.00   26
 34  \w     75.00 132.00   1.00    1.00    --  104.49  61.00 -30.00   57
 35  \w     76.00 172.00   1.00    1.00    --  104.49  61.00-150.00   96
 36  \w     73.00  99.00   1.00    1.00    --  104.49  77.00  30.00   26
 37  \w     78.00 105.00   1.00    1.00    --  104.49  61.00 -90.00   27
 38  \w     77.00 104.00   1.00    1.00    --  104.49  61.00 150.00   27
 39  \w     73.00  98.00   1.00    1.00    --  104.49  77.00 -90.00   25
 40  \w    118.00 175.00   1.00    1.00    --  104.49  77.00 -90.00   57
 41  \w     73.00 100.00   1.00    1.00    --  104.49  77.00  60.00   27
 42  \w     77.00 178.00   1.00    1.00    --  104.49  56.00 -15.09  101
 43  \w     75.00 101.00   1.00    1.00    --  104.49  63.00   1.13   26
;
_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      0.1940637000
_diffrn_orient_matrix_UB_12      0.0334727000
_diffrn_orient_matrix_UB_13      -0.0511382000
_diffrn_orient_matrix_UB_21      0.1018943000
_diffrn_orient_matrix_UB_22      -0.0536982000
_diffrn_orient_matrix_UB_23      0.1002243000
_diffrn_orient_matrix_UB_31      0.0063522000
_diffrn_orient_matrix_UB_32      -0.1621902000
_diffrn_orient_matrix_UB_33      -0.0438145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11161
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.695
_diffrn_reflns_theta_min         6.085
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.333
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_preparation       Purchased
_exptl_crystal_recrystallization_method 'Grown in nmr tube in C6H6'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.181
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0086(4)
_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   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0355P)^2^+0.2635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                834
_reflns_number_total             842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11895_si_002.cif
_cod_data_source_block           exp_1691
_cod_depositor_comments
'Adding full bibliography for 4133967--4133980.cif.'
_cod_database_code               4133980
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         RuC10H10
_chemical_oxdiff_usercomment     'Crystallized from C6H6'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
;
_shelx_res_checksum              87102
_shelx_hkl_checksum              14108
_olex2_date_sample_data_collection 2019-07-03
_olex2_exptl_crystal_mounting_method '0.3 um nylon loop from Hampton Research'
_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 1.630
_oxdiff_exptl_absorpt_empirical_full_min 0.709