(5<i>R</i>,6<i>R</i>,7<i>R</i>,9<i>R</i>,13<i>R</i>,14<i>S</i>)-21-Cyclopropylmethyl-6,14-<i>endo</i>-ethano-2',3',4',5',7,8-hexahydro-4',4',5',5'-tetramethylfurano[2',3'6,7]normorphide hydrochloride methanol solvate
Čejka, Jan; Kratochvíl, Bohumil; Chudík, Miloslav; Jegorov, Alexandr; Acta Crystallographica Section E 61 (2005) o2274–o2276; doi:10.1107/S1600536805019410

data_2206255
_publ_section_title
;(5<i>R</i>,6<i>R</i>,7<i>R</i>,9<i>R</i>,13<i>R</i>,14<i>S</i>)-21-Cyclopropylmethyl-6,14-<i>endo</i>-ethano-2',3',4',5',7,8-hexahydro-4',4',5',5'-tetramethylfurano[2',3'6,7]normorphide
 hydrochloride methanol solvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2274
_journal_page_last               o2276
_journal_paper_doi               10.1107/S1600536805019410
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C28 H38 N O3 +, Cl -, C H4 O'
_chemical_formula_moiety         'C28 H38 N O3 +, Cl -, C H4 O'
_chemical_formula_sum            'C29 H42 Cl N O4'
_chemical_formula_weight         504.11
_chemical_name_systematic
;
(5R,6R,7R,9R,13R,14S)-21-Cyclopropylmethyl-6,14-endo-ethano-
2',3',4',5',7,8-hexahydro-4',4',5',5'-tetramethylfurano-
[2',3'6,7]normorphide hydrochloride methanol solvate
;
_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                   11.5861(5)
_cell_length_b                   13.7665(7)
_cell_length_c                   16.8391(8)
_cell_measurement_reflns_used    16127
_cell_measurement_temperature    295
_cell_measurement_theta_max      77
_cell_measurement_theta_min      5
_cell_volume                     2685.8(2)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis RED (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.090
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29111
_diffrn_reflns_theta_full        73.787
_diffrn_reflns_theta_max         76.862
_diffrn_reflns_theta_min         4.633
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details 'Flack (1983), 1563 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.016(14)
_refine_ls_extinction_coef       219(18)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_ref   1.0818
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000329
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Weighting scheme using Chebychev polynomial (Watkin <i>et al.</i>, 1994;
Prince, 1982): W = [weight] * [1-(\DF/6*\sF)^2^]^2^; [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 (13.3 -3.19 10.8) and x= F~calc~/F~max~.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0524
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                4754
_reflns_number_total             5505
_reflns_threshold_expression     I>1.96u(I)
_cod_data_source_file            ob6533.cif
_cod_data_source_block           I
_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 1527 2010-12-29 10:47:43Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C29 H42 Cl1 N1 O4'
_cod_database_code               2206255
_cod_database_fobs_code          2206255