Facile access to imidazole and imidazolium substituted dibenzo-diazocines
Sathyanarayana, Arruri; Prabusankar, Ganesan; New Journal of Chemistry 38 (2014) 3613–; doi:10.1039/C4NJ00351A

data_7054370
_publ_section_title
;
 Facile access to imidazole and imidazolium substituted dibenzo-diazocines
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3613
_journal_paper_doi               10.1039/C4NJ00351A
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         'C33 H30 N8, 2(Cl), H2 O'
_chemical_formula_sum            'C33 H32 Cl2 N8 O'
_chemical_formula_weight         627.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2014-04-21
_audit_creation_method
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  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
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_cell_angle_alpha                84.154(8)
_cell_angle_beta                 79.178(10)
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_cell_formula_units_Z            2
_cell_length_a                   8.3442(10)
_cell_length_b                   12.5633(12)
_cell_length_c                   15.0779(16)
_cell_measurement_reflns_used    2700
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.0985
_cell_measurement_theta_min      3.5353
_cell_volume                     1543.7(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
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olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
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_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.865131
_diffrn_measured_fraction_theta_max 0.865131
_diffrn_measurement_details
;
  1 omega  -35.00   36.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   50.0000  -30.0000 71

  2 omega -101.00  -29.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000 -180.0000 72

  3 omega  -61.00   -6.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   19.0000  -30.0000 55

  4 omega  -10.00   82.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  150.0000 92

  5 omega  -14.00   72.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 86

  6 omega   36.00  120.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  -60.0000 84

  7 omega   76.00  122.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 46

  8 omega   42.00  102.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -134.0000   27.0000 60

  9 omega   56.00   86.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 30

 10 omega   43.00   78.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 35

 11 omega  103.00  129.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 26

 12 omega   76.00  107.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 31

 13 omega   89.00  132.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000    0.0000 43

 14 omega   49.00  105.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 56

 15 omega   53.00   93.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 40

 16 omega  100.00  177.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 77

 17 omega   83.00  171.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -120.0000 88

 18 omega  101.00  178.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 77

 19 omega   39.00  102.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  150.0000 63

 20 omega   47.00  141.00   1.0000    1.8300
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -30.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0314860000
_diffrn_orient_matrix_UB_12      -0.1117788000
_diffrn_orient_matrix_UB_13      0.0509762000
_diffrn_orient_matrix_UB_21      -0.0225765000
_diffrn_orient_matrix_UB_22      0.0492175000
_diffrn_orient_matrix_UB_23      0.0912090000
_diffrn_orient_matrix_UB_31      -0.1840317000
_diffrn_orient_matrix_UB_32      0.0171161000
_diffrn_orient_matrix_UB_33      -0.0002835000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8560
_diffrn_reflns_theta_full        71.237702
_diffrn_reflns_theta_max         71.24
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3458
_exptl_crystal_description       needle
_exptl_crystal_F_000             655.2367
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.544832
_refine_diff_density_min         -0.505653
_refine_diff_density_rms         0.113318
_refine_ls_d_res_high            0.814185
_refine_ls_d_res_low             12.491575
_refine_ls_goodness_of_fit_ref   1.089649
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    55
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089649
_refine_ls_R_factor_all          0.114942
_refine_ls_R_factor_gt           0.072302
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+3.3671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.224077
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3204
_reflns_number_total             5183
_reflns_threshold_expression     I>=2u(I)
_cod_duplicate_entry             7054208
_cod_data_source_file            c4nj00351a2.cif
_cod_data_source_block           7
_cod_database_code               7054370
_chemical_oxdiff_formula         'C33 H32 Cl2 N8 O'
_reflns_odcompleteness_completeness 90.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97