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_4128217
_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 H54 O4'
_chemical_formula_sum            'C48 H54 O4'
_chemical_formula_weight         694.91
_chemical_melting_point          519(2)
_chemical_name_common            'mestranol rotor'
_chemical_name_systematic
(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
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-19T15:37:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-12-04 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                   14.7106(4)
_cell_length_b                   14.7106(4)
_cell_length_c                   14.6565(7)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.31
_cell_volume                     2746.77(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44513
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.019
_diffrn_reflns_theta_min         1.743
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 2934 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7512
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.7505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.098
_reflns_number_gt                6667
_reflns_number_total             7512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11385_si_002.cif
_cod_data_source_block           ucla002a2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '244-248 C' was changed to '519(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        2746.8(2)
_cod_database_code               4128217
_shelx_res_checksum              95778
_shelx_hkl_checksum              97413