Facile One Pot Synthesis of Highly Photoresponsive Coinage Metal Selenides (Cu1.8Se and Ag2Se) Achieved Through Novel Cu and Ag Pyridylselenolates as Molecular Precursors
Karmakar, Gourab; Tyagi, Adish; Shah, Alpa Y.; Nigam, Sandeep; Wadawale, Amey; Gotluru, Kedarnath; Vats, Bal Govind; Kumar, N. Naveen; Singh, Vishal; Dalton Transactions  (2022) –; doi:10.1039/D2DT01897G

data_7710882
_publ_section_title
;
 Facile One Pot Synthesis of Highly Photoresponsive Coinage Metal
 Selenides (Cu1.8Se and Ag2Se) Achieved Through Novel Cu and Ag
 Pyridylselenolates as Molecular Precursors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01897G
_journal_year                    2022
_chemical_formula_sum            'C28 H32 Cu4 N4 Se4'
_chemical_formula_weight         994.57
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.261(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7261(3)
_cell_length_b                   15.9910(3)
_cell_length_c                   16.3017(3)
_cell_measurement_reflns_used    13482
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.6550
_cell_measurement_theta_min      2.5650
_cell_volume                     3264.39(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SuperFlip
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24753
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.538
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       Rhombohedral
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0830P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             7745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01897g2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710882
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.226
_shelx_estimated_absorpt_t_max   0.333
_oxdiff_exptl_absorpt_empirical_full_min 0.548
_oxdiff_exptl_absorpt_empirical_full_max 1.856
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              34949