Synthesis of reduced graphene oxide-based catalytic complexes for benzylamine–o-phenylenediamine oxidative coupling
Dheeraj,; Rana, Lata; Mahiya, Kuldeep; New Journal of Chemistry  (2026) –; doi:10.1039/D6NJ01022A

data_7064377
_publ_section_title
;
 Synthesis of reduced graphene oxide-based catalytic complexes for
 benzylamine--o-phenylenediamine oxidative coupling
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7247
_journal_page_last               7258
_journal_paper_doi               10.1039/D6NJ01022A
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C16 H16 Mo N2 O8, H2 O'
_chemical_formula_sum            'C16 H18 Mo N2 O9'
_chemical_formula_weight         478.26
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-11-13 deposited with the CCDC.	2026-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.6990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3289(5)
_cell_length_b                   11.9065(4)
_cell_length_c                   12.6831(4)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.42
_cell_volume                     1792.35(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35349
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.479
_diffrn_reflns_theta_min         2.423
_diffrn_source_current           1.39
_diffrn_source_power             0.0695
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_correction_T_min  0.8311
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1107 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.8932.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.9482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4518
_reflns_number_total             4784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6nj01022a2.cif
_cod_data_source_block           mrm_lr_s_1470_0m
_cod_depositor_comments
'Adding full bibliography for 7064377--7064378.cif.'
_cod_database_code               7064377
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.02
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              80436
_olex2_submission_special_instructions 'No special instructions were received'