Mimicking 2,2′:6′,2′′:6′′,2′′′-quaterpyridine complexes for the light-driven hydrogen evolution reaction: synthesis, structural, thermal and physicochemical characterizations
Rajak, Sanil; Schott, Olivier; Kaur, Prabhjyot; Maris, Thierry; Hanan, Garry S.; Duong, Adam; RSC Advances 9 (2019) 28153–; doi:10.1039/C9RA04303A

data_7233701
_publ_section_title
;
 Mimicking
 2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;:6&#x2032;&#x2032;,2&#x2032;&#x2032;&#x2032;-quaterpyridine
 complexes for the light-driven hydrogen evolution reaction: synthesis,
 structural, thermal and physicochemical characterizations
;
_journal_issue                   48
_journal_name_full               'RSC Advances'
_journal_page_first              28153
_journal_paper_doi               10.1039/C9RA04303A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C16 H16 N13 Ni O4, N O3'
_chemical_formula_sum            'C16 H16 N14 Ni O7'
_chemical_formula_weight         575.13
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-04 deposited with the CCDC.    2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.139(3)
_cell_angle_beta                 91.020(3)
_cell_angle_gamma                113.356(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6118(5)
_cell_length_b                   11.7609(6)
_cell_length_c                   14.1181(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    150
_cell_measurement_theta_max      55.056
_cell_measurement_theta_min      2.741
_cell_volume                     1456.81(14)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21341
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.837
_diffrn_reflns_theta_min         2.739
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.961
_exptl_absorpt_correction_T_max  0.3027
_exptl_absorpt_correction_T_min  0.2118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1511 before and 0.0773 after correction. The Ratio of minimum to maximum transmission is 0.6997. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       Block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
A solvent mask was calculated and 174 electrons were 
found in a volume of 438\%A^3 per unit cell.
This is consistent with the presence of 
a total of 4 DMSO per unit-cell 
and formula unit (Z=1).
;
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0052(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0691P)^2^+1.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5349
_reflns_number_total             6685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04303a2.cif
_cod_data_source_block           ada127
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2025-04-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H32 N28 Ni2 O14'
_cod_original_formula_weight         1150.27
_cod_original_formula_moiety         '2(C16 H16 N13 Ni O4), 2(N O3)'
_cod_original_formula_units_Z            1
_cod_database_code               7233701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.588
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12)
2.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B), N11(H11A,H11B), N12(H12A,H12B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              93890
_shelx_fab_checksum              17356