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_7710884
_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            'C42 H48 Ag6 N6 Se6'
_chemical_formula_weight         1757.84
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                 101.103(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1492(4)
_cell_length_b                   16.0365(5)
_cell_length_c                   13.0874(5)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8920
_cell_measurement_theta_min      2.4620
_cell_volume                     2502.10(15)
_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    'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  -8.00   0.50    2.00    --   -5.03 -62.00 -39.00   50
  2  \w    -23.00  25.00   0.50    2.00    --   -5.03 -99.00   0.00   96
  3  \w    -23.00  22.00   0.50    2.00    --   -5.03 -99.00 -60.00   90
  4  \w    -20.00  28.00   0.50    2.00    --   -5.03 -99.00 -90.00   96
  5  \w    -12.00  27.00   0.50    2.00    --   -5.03 -99.00-180.00   78
  6  \w    -17.00  68.00   0.50    2.00    --   -5.03  62.00  98.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0412878000
_diffrn_orient_matrix_UB_12      -0.0281888000
_diffrn_orient_matrix_UB_13      -0.0254738000
_diffrn_orient_matrix_UB_21      -0.0071944000
_diffrn_orient_matrix_UB_22      -0.0156509000
_diffrn_orient_matrix_UB_23      0.0489723000
_diffrn_orient_matrix_UB_31      -0.0422687000
_diffrn_orient_matrix_UB_32      0.0302629000
_diffrn_orient_matrix_UB_33      0.0015404000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24811
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.072
_diffrn_reflns_theta_min         2.032
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34356
_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            colourless
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5012
_reflns_number_total             6466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01897g2.cif
_cod_data_source_block           shelx_CCDC2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710884
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.554
_shelx_estimated_absorpt_t_max   0.730
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_exptl_absorpt_empirical_full_max 2.294
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01ae5740171b335607ac285b431751975a000264f3c
;
_diffrn_oxdiff_digest_hkl
;
013e938793f0b4f23369d376b99429fe07a305
;
_shelx_res_checksum              34401