Crystal structure of 1-hydroxymethyl-10α-methoxy-9,10-dihydrolysergol, C~18~H~24~N~2~O~3~
J. Cejka; B. Kratochvíl; L. Cvak; A. Jegorov; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 351–352; doi:

data_8101793
_publ_section_title
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Crystal structure of 1-hydroxymethyl-10\a-methoxy-9,10-dihydrolysergol, 
C~18~H~24~N~2~O~3~
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              351
_journal_page_last               352
_journal_volume                  220
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H24 N2 O3'
_chemical_formula_sum            'C18 H24 N2 O3'
_chemical_formula_weight         316.40
_chemical_name_systematic
1-hydroxymethyl-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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8679(10)
_cell_length_b                   10.8765(10)
_cell_length_c                   15.458(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293
_cell_measurement_theta_max      50
_cell_measurement_theta_min      48
_cell_volume                     1659.1(3)
_computing_cell_refinement       'CAD-4 software [9]'
_computing_data_collection       'CAD-4 software [9]'
_computing_data_reduction        'RC93 [10]'
_computing_molecular_graphics    'ORTEP3 [13]'
_computing_publication_material  'CRYSTALS [12]'
_computing_structure_refinement  'CRYSTALS [12]'
_computing_structure_solution    'SIR92 [11]'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  3.990
_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            3615
_diffrn_reflns_theta_full        66.629
_diffrn_reflns_theta_max         74.864
_diffrn_reflns_theta_min         4.972
_diffrn_standards_decay_%        1.21
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_T_min  0.8227
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Azimutal absorption correction [6]'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.56
_refine_ls_abs_structure_details 'Flack, 3293 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000293
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, [7,8] 
 [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 [8] 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.51 4.66 5.74 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0802
_refine_ls_wR_factor_gt          0.0794
_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                3198
_reflns_number_total             3293
_reflns_threshold_expression     I>2sigma(I)
_oxford_diffrn_Wilson_B_factor   2.06
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_scale          3.961(13)
_cod_data_source_file            1267-1549.cff
_cod_data_source_block           cejka20005-11-05_HMDL
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
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_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               8101793