Nickel–PNN catalysed sustainable synthesis of polysubstituted quinolines under microwave irradiation
Mohite, Manali A.; Sheokand, Sonu; Balakrishna, Maravanji S.; Catalysis Science & Technology 14 (2024) 5959–5969; doi:10.1039/D4CY00863D

data_1573002
_publ_section_title
;
 Nickel--PNN catalysed sustainable synthesis of polysubstituted quinolines
 under microwave irradiation
;
_journal_issue                   20
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5959
_journal_page_last               5969
_journal_paper_doi               10.1039/D4CY00863D
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C25 H20 Cl N5 Ni P, C F3 O3 S'
_chemical_formula_sum            'C26 H20 Cl F3 N5 Ni O3 P S'
_chemical_formula_weight         664.66
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            36
_cell_length_a                   42.930(3)
_cell_length_b                   42.930(3)
_cell_length_c                   16.9889(15)
_cell_measurement_reflns_used    8823
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.50
_cell_volume                     27116(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       '<i>APEX4</i> (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1396
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_min         1.881
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1171 before and 0.0890 after correction.
The Ratio of minimum to maximum transmission is 0.6530.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             12168
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+211.2561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6487
_reflns_number_total             10665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cy00863d2.cif
_cod_data_source_block           comp_4
_cod_depositor_comments
;

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H40 Cl2 F6 N10 Ni2 O6 P2 S2'
_cod_original_formula_weight         1329.32
_cod_original_formula_moiety         '2(C25 H20 Cl N5 Ni P), 2(C F3 O3 S)'
_cod_original_formula_units_Z            18
_cod_original_cell_volume        27115(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1573002
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N7(H7A), C7(H7), C3(H3), C2(H2A), C21(H21), C10(H10), C50(H50),
 C17(H17), C46(H46), C36(H36), C41(H41), C27(H27), C47(H47), C44(H44), C37(H37),
  C16(H16), C28(H28), C48(H48), C18(H18), C38(H38), C23(H23), C9(H9), C15(H15),
 C19(H19), C40(H40), C29(H29), C25(H25), C12(H12), C4(H4), C32(H32), C34(H34),
 C24(H24), C22(H22), C35(H35), C49(H49), C43(H43), C42(H42), C13(H13), C11(H11)
;
_shelx_res_checksum              52202
_shelx_fab_checksum              77458
_olex2_submission_special_instructions 'No special instructions were received'