Steroidal Wheel-and-Axle Host Type Molecules: Insights from Awkward Shape, Conformation,Z′ > 1 and Packing
Ramirez-Montes, Pedro I.; Ochoa, María E.; Santillan, Rosa; Ramírez, Daniel J.; Farfán, Norberto; Crystal Growth & Design 14 (2014) 4681–; doi:10.1021/cg500772f

data_4511731
_publ_section_title
;
 Steroidal Wheel-and-Axle Host Type Molecules: Insights from Awkward
 Shape, Conformation,Z&#x2032; &gt; 1 and Packing
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4681
_journal_paper_doi               10.1021/cg500772f
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H52 F2 O4'
_chemical_formula_sum            'C46 H52 F2 O4'
_chemical_formula_weight         706.87
_chemical_melting_point          463.6(5)
_chemical_name_systematic
;
1,4-bis(17?-hydroxy-17?-ethynyl-4-estren-3-one)-2,3-difluorobenzene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-05-19
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.0000
_cell_angle_beta                 125.1400(22)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   21.20580(70)
_cell_length_b                   17.47010(110)
_cell_length_c                   17.11290(80)
_cell_measurement_reflns_used    12777
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     5184.3(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.006148
_diffrn_orient_matrix_UB_12      0.026066
_diffrn_orient_matrix_UB_13      0.056036
_diffrn_orient_matrix_UB_21      0.001454
_diffrn_orient_matrix_UB_22      0.050797
_diffrn_orient_matrix_UB_23      -0.025857
_diffrn_orient_matrix_UB_31      -0.05732
_diffrn_orient_matrix_UB_32      0.004085
_diffrn_orient_matrix_UB_33      -0.036024
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28807
_diffrn_reflns_point_group_measured_fraction_full 0.97
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         24.981
_diffrn_reflns_theta_min         3.849
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  1.0049
_exptl_absorpt_correction_T_min  0.9528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Please see the response for PLAT606 at the beginning of the CIF
;
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1999
_refine_ls_R_factor_gt           0.106
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1942P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2651
_refine_ls_wR_factor_ref         0.3298
_reflns_number_gt                4383
_reflns_number_total             8878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            compound_5.cif
_cod_data_source_block           NOR_2F_SAN643
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '
463.15 - 464.15' was changed to
'463.6(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511730--4511732.cif.
;
_cod_original_cell_volume        5184.337(462)
_cod_database_code               4511731