Crystal structure of 1-methyl-10α-methoxy-9,10-dihydrolysergol, C~18~H~24~N~2~O~2~
Cejka, J.; Kratochvíl, B.; Cvak, L.; Jegorov, A.; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 207–208; doi:

data_8101748
_publ_section_title
;
Crystal structure of 1-methyl-10\a-methoxy-9,10-dihydrolysergol, 
C~18~H~24~N~2~O~2~
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              207
_journal_page_last               208
_journal_volume                  220
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_compound_source        'IVAX Pharmaceuticals, Czech Republic'
_chemical_formula_moiety         'C18 H24 N2 O2'
_chemical_formula_sum            'C18 H24 N2 O2'
_chemical_formula_weight         300.40
_chemical_name_systematic        1-methyl-10\a-methoxy-9,10-dihydrolysergol
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-02-11
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8053(7)
_cell_length_b                   10.9184(8)
_cell_length_c                   15.3758(15)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293
_cell_measurement_theta_max      50
_cell_measurement_theta_min      48
_cell_volume                     1646.1(2)
_computing_cell_refinement
;
 CAD-4 software (Enraf-Nonius, 1989) 
;
_computing_data_collection
;
 CAD-4 software (Enraf-Nonius, 1989) 
;
_computing_data_reduction
;
 RC93 (Watkin, Prout & Lilley, 1994) 
;
_computing_molecular_graphics
;
 ORTEP3 (Farrugia, 1997)
;
_computing_publication_material
;
 CRYSTALS (Bettridge et al 2003) 
;
_computing_structure_refinement
;
 CRYSTALS (Bettridge et al 2003) 
;
_computing_structure_solution
;
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Enraf-Nonius CAD4 
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  2.339
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3803
_diffrn_reflns_theta_full        74.905
_diffrn_reflns_theta_max         74.905
_diffrn_reflns_theta_min         4.968
_diffrn_standards_decay_%        0.70
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.8763
_exptl_absorpt_correction_T_min  0.8572
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack, 3392 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.11(15)
_refine_ls_extinction_coef       980(40)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000129
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are:  3.42 1.97 2.61 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0457
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0449
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3309
_reflns_number_total             3392
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          5.009(13)
_oxford_structure_analysis_title 'MELUOL MECN CEJKA 970708'
_cod_data_source_file            1267-1489.cff
_cod_data_source_block           CRYSTALS_MELUOL
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               8101748
_reflns_number_all               3392