Throwing in a Monkey Wrench to Test and Determine Geared Motion in the Dynamics of a Crystalline One-Dimensional (1D) Columnar Rotor Array.
Pérez-Estrada, Salvador; Rodríguez-Molina, Braulio; Maverick, Emily F.; Khan, Saeed I.; Garcia-Garibay, Miguel A; Journal of the American Chemical Society 141 (2019) 2413–2420; doi:10.1021/jacs.8b11385

data_4128218
_publ_section_title
;
 Throwing in a Monkey Wrench to Test and Determine Geared Motion in the
 Dynamics of a Crystalline One-Dimensional (1D) Columnar Rotor Array.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2413
_journal_page_last               2420
_journal_paper_doi               10.1021/jacs.8b11385
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration
' by relation to a reference structure (mestranol)'
_chemical_formula_moiety         'C48 H53.60 F0.40 O4'
_chemical_formula_sum            'C48 H53.6 F0.4 O4'
_chemical_formula_weight         702.11
_chemical_melting_point          500(2)
_chemical_name_common
'Solid solution 1(1-x)2x, x=0.2 where 1 is the mestranol rotor and 2 is the difluoromestranol rotor'
_chemical_name_systematic
'Solid solution of (8R,8'R,9S,9'S,13S,13'S,14S,14'S,17S,17'S)-17,17'-(1,4-phenylenebis(ethyne-2,1-diyl))bis(3-methoxy-13-methyl-7,8,9,11,12,13,14,15,16,17-decahydro-6H-cyclopenta[a]phenanthren-17-ol (80%) and solute, same compound containing 2,3-difluorophenylene, (20%)'
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-12-14 deposited with the CCDC.
2019-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.758(4)
_cell_length_b                   14.758(4)
_cell_length_c                   14.683(4)
_cell_measurement_reflns_used    5501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      3.92
_cell_volume                     2769.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35625
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.407
_diffrn_reflns_theta_min         3.915
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.9146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9256
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0488P)^2^+0.5565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                7279
_reflns_number_total             9256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11385_si_003.cif
_cod_data_source_block           gg2711s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '225-229 \%C' was changed to '500(2)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2769.7(15)
_cod_original_formula_sum        'C48 H53.60 F0.40 O4'
_cod_database_code               4128218
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2014/6
_shelx_res_checksum              11099
_shelx_hkl_checksum              28720