Synthesis of novel 1-methylindole trimer and tetramer under Friedel–Crafts reaction conditions and determination of their structures by X-ray crystallography
Mahato, Shashi B.; Garai, Subhadra; Weber, Manuela; Luger, Peter; Journal of the Chemical Society, Perkin Transactions 1  (2000) 2767–; doi:10.1039/b002074p

data_7213319
_publ_contact_author
;
     Prof. Peter Luger
     Institut f\"ur Chemie/Kristallographie
     Freie Universit\"at Berlin
     Fachbereich Biologie, Chemie, Pharmazie
     Takustr. 6
     14195 Berlin
     Germany
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_publ_section_title
;
 Synthesis of novel 1-methylindole trimer and tetramer under
 Friedel--Crafts reaction conditions and determination of their structures
 by X-ray crystallography
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2767
_journal_paper_doi               10.1039/b002074p
_journal_year                    2000
_chemical_formula_moiety         'C28 H25 N3'
_chemical_formula_sum            'C28 H25 N3'
_chemical_formula_weight         403.51
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2b 2a'
_symmetry_space_group_name_H-M   'P 21 a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   9.527(2)
_cell_length_b                   12.367(5)
_cell_length_c                   18.594(7)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      20
_cell_volume                     2190.8(13)
_computing_cell_refinement       'STOE software'
_computing_data_collection       'STOE software'
_computing_data_reduction        'Stoe-routine REDUC'
_computing_molecular_graphics
;
SCHAKAL88 (Keller, 1988); ORTEPII (Johnson, 1976)
;
_computing_publication_material
;
SHELXL-93_ACTA (Sheldrick, 1993)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
; 
Stoe four circle diffractometer, microVAX controlled
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  no
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2058
_diffrn_reflns_theta_full        67.06
_diffrn_reflns_theta_max         67.06
_diffrn_reflns_theta_min         4.29
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_type   no
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(11)
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         2058
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.3713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                1613
_reflns_number_total             2058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002074psup1.cif
_cod_data_source_block           in2
_cod_depositor_comments
;
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 
;
_cod_original_sg_symbol_H-M      'P 21ab'
_cod_database_code               7213319