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_7247800
_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(I), C21 H23 N5 O2, H2 O'
_chemical_formula_sum            'C21 H25 I2 N5 O3'
_chemical_formula_weight         649.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 110.401(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8789(13)
_cell_length_b                   10.7830(9)
_cell_length_c                   15.3311(11)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.33
_cell_volume                     2460.4(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4582
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.707
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1173 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.8118.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.480
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0880
_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^)+(0.1577P)^2^+34.7324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2703
_refine_ls_wR_factor_ref         0.2946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3651
_reflns_number_total             4582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra06477h2.cif
_cod_data_source_block           2d_komal_naveedzafar_qau_0ma_a_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               7247800
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.893(3)
 0.107(3)
2. 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 C(H,H,H) groups, All O(H,H) groups
3.a Free rotating group:
 O3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C6(H6), C12(H12), C18(H18), C7(H7), C3(H3), C10(H10), C4(H4A),
  C19(H19), C11(H11), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.492
_shelx_estimated_absorpt_t_max   0.600
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device'
_shelx_res_checksum              82439