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_4511730
_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         'C48 H58 O4, C2 H3 N1'
_chemical_formula_sum            'C50 H61 N O4'
_chemical_formula_weight         740.00
_chemical_melting_point          469.6(5)
_chemical_name_systematic
;
1,4-bis[4-estren-17?-ethynyl-18a-homo-17?-ol-3-one]-benzene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                 100.9196(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.52420(20)
_cell_length_b                   13.47900(29)
_cell_length_c                   23.94720(50)
_cell_measurement_reflns_used    71366
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     4286.36(14)
_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      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      0.042257
_diffrn_orient_matrix_UB_12      -0.057641
_diffrn_orient_matrix_UB_13      0.016441
_diffrn_orient_matrix_UB_21      0.061149
_diffrn_orient_matrix_UB_22      0.043295
_diffrn_orient_matrix_UB_23      0.006212
_diffrn_orient_matrix_UB_31      -0.012083
_diffrn_orient_matrix_UB_32      0.017525
_diffrn_orient_matrix_UB_33      0.038727
_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  0.065
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65427
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_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        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.0343
_exptl_absorpt_correction_T_min  0.9565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.073(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         17445
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0938
_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^)+(0.0840P)^2^+2.3847P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.232
_reflns_number_gt                11609
_reflns_number_total             17445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            compound_3.cif
_cod_data_source_block           LEVO_2H_SAN617
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '
469.15 - 470.15' was changed to
'469.6(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        4286.359(146)
_cod_database_code               4511730