Synthesis, Characterization, and Solid State Dynamic Studies of a Hydrogen Bond-Hindered Steroidal Molecular Rotor with a Flexible Axis.
Mayorquín-Torres, Martha C; Colin-Molina, Abraham; Pérez-Estrada, Salvador; Galano, Annia; Rodríguez-Molina, Braulio; Iglesias-Arteaga, Martín A; The Journal of organic chemistry 83 (2018) 3768–3779; doi:10.1021/acs.joc.8b00134

data_4035468
_publ_contact_author
;
      'Braulio Rodr\'iguez-Molina'
      Instituto de Q\'imica,
      Universidad Aut\'onoma de M\'exico,
      Circuito Exterior,
      Cuidad Universitaria.
      04510 Ciudad de M\'exico
      M\'exico  
      
;
_publ_section_title
;
 Synthesis, Characterization, and Solid State Dynamic Studies of a
 Hydrogen Bond-Hindered Steroidal Molecular Rotor with a Flexible Axis.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3768
_journal_page_last               3779
_journal_paper_doi               10.1021/acs.joc.8b00134
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C60 H82 O6'
_chemical_formula_weight         899.25
_space_group_crystal_system      monoclinic
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_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90.4710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   52.9571(12)
_cell_length_b                   8.5386(2)
_cell_length_c                   11.2085(3)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.65
_cell_measurement_theta_min      4.27
_cell_volume                     5068.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0216
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_diffrn_reflns_limit_k_min       -10
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.777
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 3736 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9147
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0531P)^2^+1.1527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.842
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                9026
_reflns_number_total             9147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00134_si_002.cif
_cod_data_source_block           cu_063RMB17_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4035468
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              7317
_shelx_hkl_checksum              39545