Z’=2 crystallization of the three isomeric piridinoylhydrazone derivatives of isosteviol: Inclusion of an “extra” molecule in a unitcell as a “cost” of transferring a robust mirror-symmetrical H-bonding motif from an racemic environment into a homochiral one
Lodochnikova, Olga; Dobrynin, Alexey B.; Andreeva, Olga V.; Strobykina, Irina Yu; Kataev, Vladimir E.; Litvinov, Igor; CrystEngComm  (2014) –; doi:10.1039/c4ce00173g

data_7214368
_publ_section_title
;
 Z&#x2019;=2 crystallization of the three isomeric piridinoylhydrazone
 derivatives of isosteviol: Inclusion of an &#x201C;extra&#x201D; molecule
 in a unitcell as a &#x201C;cost&#x201D; of transferring a robust
 mirror-symmetrical H-bonding motif from an racemic environment into a
 homochiral one
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/c4ce00173g
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H37 N3 O3'
_chemical_formula_sum            'C27 H37 N3 O3'
_chemical_formula_weight         451.60
_chemical_melting_point          518
_chemical_name_systematic
;Methyl 16-[N'-(pyridin-3-ylcarbonyl)hydrazono]-
ent-beyeran-19-oate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.608(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.966(3)
_cell_length_b                   19.688(6)
_cell_length_c                   15.559(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2437.7(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1385
_diffrn_reflns_av_sigmaI/netI    0.3154
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22443
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9960
_exptl_absorpt_correction_T_min  0.9841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         11580
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.2761
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1777
_reflns_number_gt                3693
_reflns_number_total             11580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00173g1.cif
_cod_data_source_block           k119_fin2
_cod_original_cell_volume        2437.6(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7214368