Graphite oxide: a metal free highly efficient carbocatalyst for the synthesis of 1,5-benzodiazepines under room temperature and solvent free heating conditions
Jamatia, Ramen; Gupta, Ajay; Dam, Binoyargha; Saha, Mithu; Pal, Amarta Kumar; Green Chem. 19 (2017) 1576–; doi:10.1039/C6GC03110B

data_7227670
_publ_section_title
;
 Graphite oxide: a metal free highly efficient carbocatalyst for the
 synthesis of 1,5-benzodiazepines under room temperature and solvent free
 heating conditions
;
_journal_issue                   6
_journal_name_full               'Green Chem.'
_journal_page_first              1576
_journal_paper_doi               10.1039/C6GC03110B
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C23 H21 Cl N2'
_chemical_formula_sum            'C23 H21 Cl N2'
_chemical_formula_weight         360.89
_chemical_name_systematic        RJ-17
_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'
_atom_sites_solution_primary     iterative
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2016-10-18 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                104.148(7)
_cell_angle_beta                 102.007(6)
_cell_angle_gamma                92.918(6)
_cell_formula_units_Z            2
_cell_length_a                   6.0657(4)
_cell_length_b                   11.6494(10)
_cell_length_c                   14.2527(12)
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    296.9(6)
_cell_measurement_theta_max      27.2570
_cell_measurement_theta_min      3.9000
_cell_volume                     949.69(14)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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CrysAlisPro, Agilent Technologies,
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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
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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_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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_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      296.9(6)
_diffrn_detector_area_resol_mean 8.0640
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.8620
_diffrn_measurement_details
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  1 omega  -38.00   13.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -      -20.2184  -77.0000  120.0000 51

  2 omega  -10.00   17.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -      -20.2184  -99.0000    0.0000 27

  3 omega  -48.00   46.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -       22.4059  -57.0000 -150.0000 94

  4 omega    0.00   89.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -       22.4059   57.0000    0.0000 89

  5 omega  -30.00   -3.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -       22.4059  -57.0000   60.0000 27

  6 omega   66.00  100.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -       22.4059  178.0000 -180.0000 34

  7 omega  -45.00   32.00   1.0000    6.2100
omega____ theta____ kappa____ phi______ frames
    -       22.4059  -37.0000   90.0000 77
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0008045000
_diffrn_orient_matrix_UB_12      -0.0454527000
_diffrn_orient_matrix_UB_13      -0.0435234000
_diffrn_orient_matrix_UB_21      -0.0116673000
_diffrn_orient_matrix_UB_22      -0.0437928000
_diffrn_orient_matrix_UB_23      0.0260592000
_diffrn_orient_matrix_UB_31      -0.1196766000
_diffrn_orient_matrix_UB_32      -0.0022334000
_diffrn_orient_matrix_UB_33      -0.0143051000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6931
_diffrn_reflns_theta_full        28.721783
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.2619
_exptl_crystal_description       block
_exptl_crystal_F_000             380.4239
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.374788
_refine_diff_density_min         -0.348616
_refine_diff_density_rms         0.066045
_refine_ls_d_res_high            0.739486
_refine_ls_d_res_low             6.728731
_refine_ls_goodness_of_fit_ref   1.047577
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047577
_refine_ls_R_factor_all          0.084562
_refine_ls_R_factor_gt           0.056699
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.2247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.138382
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              14
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2999
_reflns_number_total             4235
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6gc03110b2.cif
_cod_data_source_block           RJ-17
_cod_depositor_comments          'Adding full bibliography for 7227670.cif.'
_cod_database_code               7227670
_chemical_oxdiff_formula         C23H21ClN2
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32