An efficient copper-catalyzed synthesis of hexahydro-1H- phenothiazines
Prasad, D. J. C.; Sekar, Govindasamy; Organic & Biomolecular Chemistry 7 (2009) 5091–5097; doi:10.1039/b916664e

data_7153552
_publ_section_title
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 An efficient copper-catalyzed synthesis of hexahydro-1H- phenothiazines
;
_journal_issue                   24
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              5091
_journal_page_last               5097
_journal_paper_doi               10.1039/b916664e
_journal_volume                  7
_journal_year                    2009
_chemical_formula_moiety         'C20 H23 N O2 S2'
_chemical_formula_sum            'C20 H23 N O2 S2'
_chemical_formula_weight         373.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.05(3)
_cell_angle_beta                 92.13(3)
_cell_angle_gamma                92.44(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6290(15)
_cell_length_b                   11.646(2)
_cell_length_c                   11.722(2)
_cell_measurement_reflns_used    3777
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.68
_cell_volume                     940.9(4)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX II,Bruker,2004'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
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_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15094
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.88
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.9350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.23
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_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.449
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_refine_ls_number_reflns         5309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1750
_reflns_number_gt                3377
_reflns_number_total             5309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b916664esup1.cif
_cod_data_source_block           djn-ii-45
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        940.9(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7153552