(1<i>R</i>*,3<i>R</i>*,4<i>S</i>*)-4-(<i>tert</i>-Butyldiphenylsilyloxy)-6,7-dimethoxy-1-methyl-3-phenyl-1,2,3,4-tetrahydroisoquinoline
Pizarro, J. L.; Arriortua, M. I.; Tellitu, I.; Badía, D.; Domínguez, E.; Ochando, L.; Amigó, J. M.; Debaerdemaeker, T.; Acta Crystallographica Section C 53 (1997) 355–358; doi:10.1107/S0108270196013376

data_2005962
_publ_contact_author
;
   Dr. Jos\'e Luis Pizarro
   Dpto. de Mineralog\'ia y Petrolog\'ia
   Universidad del Pa\'is Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_section_title
(1<i>R</i>*,3<i>R</i>*,4<i>S</i>*)-4-(<i>tert</i>-Butyldiphenylsilyloxy)-6,7-dimethoxy-1-methyl-3-phenyl-1,2,3,4-tetrahydroisoquinoline
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              355
_journal_page_last               358
_journal_paper_doi               10.1107/S0108270196013376
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C34 H39 N O3 Si'
_chemical_formula_sum            'C34 H39 N O3 Si'
_chemical_formula_weight         537.773
_chemical_name_systematic
;
   (1R*,3R*,4S*)-4-Tert-Butyldiphenylsilyloxy-6,7-dimethoxy-1-
   methyl-3-phenyl-1,2,3,4-tetrahydroisoquinoline.
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.181(3)
_cell_length_b                   21.020(4)
_cell_length_c                   17.402(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      9
_cell_volume                     2992.5(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'Xtal3.2 (Hall, Flack & Stewart, 1992)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'PARST (Nardelli, 1983), SHELXL93'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.008
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2794
_diffrn_reflns_theta_max         27.26
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.225
_refine_ls_abs_structure_details 'Flack (1983) = 0.08(13)'
_refine_ls_abs_structure_Flack   0.08(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.121
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment
'H atoms riding on C atoms [U~iso~(H) = 1.2U~eq~(C)]'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.208
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_obs          0.0305
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.4280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0925
_refine_ls_wR_factor_obs         0.0829
_reflns_number_observed          2473
_reflns_number_total             2643
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1410.cif
_cod_data_source_block           compound_AMI50
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.4280P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.4280P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2992.0(10)
_cod_database_code               2005962