Synthesis, crystal structure, characterization of pyrazine diaminotriazine based complexes and their systematic comparative study with pyridyl diaminotriazine based complexes for light-driven hydrogen production
Rajak, Sanil; Schott, Olivier; Kaur, Prabhjyot; Maris, Thierry; Hanan, Gary S.; Duong, Adam; Polyhedron 180 (2020) 114412–; doi:10.1016/j.poly.2020.114412

data_1559880
_publ_section_title
;
 Synthesis, crystal structure, characterization of pyrazine
 diaminotriazine based complexes and their systematic comparative study
 with pyridyl diaminotriazine based complexes for light-driven hydrogen
 production
;
_journal_name_full               Polyhedron
_journal_page_first              114412
_journal_paper_doi               10.1016/j.poly.2020.114412
_journal_volume                  180
_journal_year                    2020
_chemical_formula_moiety         'C14 H14 Cu N15 O3, N O3'
_chemical_formula_sum            'C14 H14 Cu N16 O6'
_chemical_formula_weight         565.95
_chemical_name_systematic
;
(nitrato)-bis[6-(pyrazin-2-yl)-1,3,5-triazine-2,4-diamine]-copper(ii) nitrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                93.120(2)
_cell_angle_beta                 96.497(2)
_cell_angle_gamma                97.972(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3550(4)
_cell_length_b                   10.4080(5)
_cell_length_c                   12.2948(5)
_cell_measurement_reflns_used    5190
_cell_measurement_temperature    100
_cell_measurement_theta_max      52.199
_cell_measurement_theta_min      3.156
_cell_volume                     1049.33(8)
_computing_cell_refinement
;
SAINT (2013) V8.37A; 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) V8.37A; 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      100
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3582
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        52.238
_diffrn_reflns_theta_max         52.238
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    6.058
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 34764 reflections, Rint = 0.0681
 (29284 with I > 3sig(I), Rint = 0.0667)
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       Frgament
_exptl_crystal_F_000             574
_exptl_crystal_recrystallization_method 'crystallized from MeOH/H2O'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.0094(14)
_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   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1219P)^2^+0.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3410
_reflns_number_total             3582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rm196.cif
_cod_data_source_block           rm196
_cod_database_code               1559880
_cod_database_fobs_code          1559880