Palladium-anchored donor-flexible pyridylidene amide (PYA) electrocatalysts for CO2 reduction
Khurshid, Afshan; Tanveer, Tania; Hafeez, Komal; Ahmed, Maqsood; Akhtar, Zareen; Zafar, M. Naveed; RSC Advances 13 (2023) 34817–34825; doi:10.1039/D3RA06477H

data_7247802
_publ_section_title
;
 Palladium-anchored donor-flexible pyridylidene amide (PYA)
 electrocatalysts for CO2 reduction
;
_journal_issue                   49
_journal_name_full               'RSC Advances'
_journal_page_first              34817
_journal_page_last               34825
_journal_paper_doi               10.1039/D3RA06477H
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         '2(Cl), C31 H27 N5 O2, H2 O'
_chemical_formula_sum            'C31 H29 Cl2 N5 O3'
_chemical_formula_weight         590.513
_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_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2023-07-15
_audit_creation_method
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-07-15 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                91.744(1)
_cell_angle_beta                 101.920(2)
_cell_angle_gamma                109.870(1)
_cell_formula_units_Z            2
_cell_length_a                   9.2037(4)
_cell_length_b                   11.6728(5)
_cell_length_c                   14.0506(6)
_cell_measurement_reflns_used    850
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.26
_cell_volume                     1380.69(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device       'Four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.9968
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39400
_diffrn_reflns_point_group_measured_fraction_full 0.9968
_diffrn_reflns_point_group_measured_fraction_max 0.9961
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1660 before and 0.0989 after correction.
The Ratio of minimum to maximum transmission is 0.6743.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             616.946
_refine_diff_density_max         2.8026
_refine_diff_density_min         -1.5084
_refine_diff_density_rms         0.1280
_refine_ls_d_res_high            0.7991
_refine_ls_d_res_low             9.0216
_refine_ls_goodness_of_fit_ref   1.0674
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    55
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0674
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1565P)^2^+4.0463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2561
_refine_ls_wR_factor_ref         0.2773
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4737
_reflns_number_total             5655
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ra06477h2.cif
_cod_data_source_block           1B_Komal_NavedZafar_QAU_100K_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7247802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3a,H3b)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C5(H5), C6(H6), C3(H3), C31(H31), C27(H27), C2(H2a), C1(H1),
 C17(H17), C15(H15), C16(H16), C21(H21), C30(H30), C29(H29), C11(H11), C12(H12),
  C24(H24), C23(H23), C22(H22), C28(H28), C9(H9), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device'