Synthesis and Biological Activity of Two C-7 Methyl Analogues of Vitamin D.
Sokolowska, Katarzyna; Carballa, Diego; Seoane, Samuel; Pérez-Fernández, Román; Mouriño, Antonio; Sicinski, Rafal R.; The Journal of organic chemistry 80 (2014) 165–; doi:10.1021/jo502243r

data_4030289
_publ_section_title
;
 Synthesis and Biological Activity of Two C-7 Methyl Analogues of Vitamin
 D.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              165
_journal_paper_doi               10.1021/jo502243r
_journal_volume                  80
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_formula_sum            'C27 H44.5 O3'
_chemical_formula_weight         417.13
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.2241(14)
_cell_length_b                   30.833(9)
_cell_length_c                   32.125(10)
_cell_measurement_reflns_used    2189
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.5140
_cell_measurement_theta_min      1.8269
_cell_volume                     7156(3)
_computing_cell_refinement
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'WINGX, MERCURY, ORTEP'
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 8.4441
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Opal'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2296
_diffrn_reflns_av_sigmaI/netI    0.2811
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38026
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.018
_platon_squeeze_details
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;
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.201
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     279
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.2499
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2433
_refine_ls_wR_factor_ref         0.3113
_reflns_number_gt                2152
_reflns_number_total             6323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502243r_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 4030289.cif.'
_cod_original_formula_sum        'C27 H44.50 O3'
_cod_database_code               4030289