2-(2-Chloroacetyl)-6,7-dimethoxy-1-(phenoxymethyl)-1,2,3,4-tetrahydroisoquinoline
Zhi-Hong Zou; Yong Ling; Wen-Long Huang; Acta Crystallographica Section E 63 (2007) o1596–o1597; doi:10.1107/S1600536807009476

data_2212926
_publ_section_title
2-(2-Chloroacetyl)-6,7-dimethoxy-1-(phenoxymethyl)-1,2,3,4-tetrahydroisoquinoline
_journal_coeditor_code           HK2202
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1596
_journal_page_last               o1597
_journal_paper_doi               10.1107/S1600536807009476
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H22 Cl N O4'
_chemical_formula_moiety         'C20 H22 Cl N O4'
_chemical_formula_sum            'C20 H22 Cl N O4'
_chemical_formula_weight         375.84
_chemical_melting_point          400(2)
_chemical_name_systematic
;
2-(2-Chloroacetyl)-6,7-dimethoxy-1-(phenoxymethyl)-1,2,3,4-
tetrahydroisoquinoline
;
_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           SHELXL97
_cell_angle_alpha                93.69(3)
_cell_angle_beta                 107.82(3)
_cell_angle_gamma                111.10(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7110(17)
_cell_length_b                   9.6550(19)
_cell_length_c                   12.668(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     927.9(5)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3881
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_correction_T_min  0.9133
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.264
_refine_ls_extinction_coef       0.036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                2586
_reflns_number_total             3629
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2202.cif
_cod_data_source_block           I
_cod_database_code               2212926
_cod_database_fobs_code          2212926