Synthesis of steroidal molecular compasses: exploration of the controlled assembly of solid organic materials
Aguilar-Valdez, Nancy; Maldonado-Domínguez, Mauricio; Arcos-Ramos, Rafael; Romero-Ávila, Margarita; Santillan, Rosa; Farfán, Norberto; CrystEngComm 19 (2017) 1771–; doi:10.1039/C7CE00157F

data_7227747
_publ_section_title
;
 Synthesis of steroidal molecular compasses: exploration of the controlled
 assembly of solid organic materials
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1771
_journal_paper_doi               10.1039/C7CE00157F
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H62 N2 O4'
_chemical_formula_sum            'C48 H62 N2 O4'
_chemical_formula_weight         731.00
_chemical_melting_point          483
_chemical_name_systematic
;
2,5-Bis(17alpha-ethynyl-5delta-androst-2-en-17beta-ol)-4-nitroaniline
;
_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
_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             2016-11-10T18:07:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-01-05 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.169(8)
_cell_length_b                   7.5511(15)
_cell_length_c                   16.702(3)
_cell_measurement_reflns_used    33563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4919.1(17)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_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_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.023747
_diffrn_orient_matrix_UB_12      -0.004474
_diffrn_orient_matrix_UB_13      -0.017234
_diffrn_orient_matrix_UB_21      0.009559
_diffrn_orient_matrix_UB_22      -0.000887
_diffrn_orient_matrix_UB_23      0.057574
_diffrn_orient_matrix_UB_31      -0.000868
_diffrn_orient_matrix_UB_32      -0.132249
_diffrn_orient_matrix_UB_33      0.000197
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27259
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.97
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.641
_diffrn_reflns_theta_min         4.615
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             1584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2:Hexanes'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -2(3)
_refine_ls_extinction_coef       0.019(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1601P)^2^+0.2279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2242
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.87
_reflns_Friedel_fraction_full    0.98
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                5624
_reflns_number_total             10522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00157f2.cif
_cod_data_source_block           Steroidal_compass_11
_cod_depositor_comments
;
Adding full bibliography for 7227747--7227748.cif.

2018-02-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4918.9(17)
_cod_original_formula_sum        'C24 H31 N O2'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     365.50
_cod_database_code               7227747
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              72797
_shelx_fab_checksum              45688