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_7233700
_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 H14 Cu N13 O3, N O3, 0.5(C4 H8 O), 0.5(O)'
_chemical_formula_sum            'C18 H18 Cu N14 O7'
_chemical_formula_weight         606.00
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 102.018(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1245(3)
_cell_length_b                   15.8382(4)
_cell_length_c                   21.6268(6)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.793
_cell_measurement_theta_min      3.637
_cell_volume                     3391.93(16)
_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    'ShelXT (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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49606
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.825
_diffrn_reflns_theta_min         3.032
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0689 after correction. The Ratio of minimum to maximum transmission is 0.7903. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0039(4)
_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   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7797
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1239P)^2^+5.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7080
_reflns_number_total             7797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04303a2.cif
_cod_data_source_block           ada125
_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 
;
_cod_database_code               7233700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.566
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C1C-C2C \\sim C2C-C3C \\sim C3C-C4C
 with sigma of 0.02
 O1C-C1C \\sim O1C-C4C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2B)
4. Others
 Sof(O2B)=1-FVAR(1)
 Sof(O2A)=FVAR(1)
 Fixed Sof: C1C(0.5) H1CA(0.5) H1CB(0.5) C4C(0.5) H4CA(0.5) H4CB(0.5) O1C(0.5)
 O5C(0.5) C2C(0.5) H2CA(0.5) H2CB(0.5) C3C(0.5) H3CA(0.5) H3CB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1C(H1CA,H1CB), C4C(H4CA,H4CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12)
5.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B), N11(H11A,H11B), N12(H12A,H12B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 328 electrons were 
found in a volume of 1146\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 
a total of 7.8 DMSO (328 electrons) per unit, 
so around 2 DMSO per formula unit.
;
_shelx_res_checksum              31545
_shelx_fab_checksum              25877
_olex2_submission_special_instructions 'No special instructions were received'