Graphite oxide catalyzed one-pot synthesis of highly functionalized spirodibenzo[1,4]diazepine derivatives in aqueous ethanol medium
Sarkar, Rajib; Dam, Binoyargha; Kyndiah, Lenida; Sarkar, Fillip Kumar; Gajurel, Sushmita; Pal, Amarta Kumar; Green Chemistry 24 (2022) 5579–5591; doi:10.1039/D2GC00194B

data_7245081
_publ_section_title
;
 Graphite oxide catalyzed one-pot synthesis of highly functionalized
 spirodibenzo[1,4]diazepine derivatives in aqueous ethanol medium
;
_journal_issue                   14
_journal_name_full               'Green Chemistry'
_journal_page_first              5579
_journal_page_last               5591
_journal_paper_doi               10.1039/D2GC00194B
_journal_volume                  24
_journal_year                    2022
_chemical_formula_sum            'C22 H23 N3 O3'
_chemical_formula_weight         377.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.873(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.921(3)
_cell_length_b                   22.128(5)
_cell_length_c                   14.966(4)
_cell_measurement_reflns_used    10546
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.029
_cell_measurement_theta_min      1.753
_cell_volume                     3912.9(17)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            80405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.069
_diffrn_reflns_theta_min         1.750
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.087
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         10174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1239P)^2^+3.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5883
_reflns_number_total             10174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc00194b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
          Adding full bibliography for 7245081.cif.

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H46 N6 O6'
_cod_original_formula_weight         754.87
_cod_original_formula_units_Z            4
_cod_original_cell_volume        3912.8(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7245081
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              58053