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_7710883
_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            'C50 H52 Ag6 N6 Se6'
_chemical_formula_weight         1857.95
_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     iterative
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-03-03 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                72.654(5)
_cell_angle_beta                 72.595(6)
_cell_angle_gamma                71.503(5)
_cell_formula_units_Z            1
_cell_length_a                   9.7820(7)
_cell_length_b                   12.4356(6)
_cell_length_c                   12.6351(8)
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5740
_cell_measurement_theta_min      2.4910
_cell_volume                     1355.33(16)
_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    'OLEX 1.2'
_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 0.836
_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     18.00  71.00   0.50    8.00    --   16.91  57.00   0.00  106
  2  \w     27.00  64.00   0.50    8.00    --   16.91 -98.00-121.00   74
  3  \w     -3.00  33.00   0.50    8.00    --  -16.60 -98.00-121.00   72
  4  \w    -16.00   9.00   0.50    8.00    --   16.91 -98.00-121.00   50
  5  \w    -19.00  67.00   0.50    8.00    --   16.91 -99.00-180.00  172
  6  \w    -43.00 -17.00   0.50    8.00    --   16.91 -77.00  30.00   52
  7  \w    -68.00  18.00   0.50    8.00    --   16.91 -37.00  90.00  172
  8  \w    -64.00   5.00   0.50    8.00    --   16.91 -19.00 120.00  138
  9  \w    -65.00   5.00   0.50    8.00    --  -16.60  98.00 -14.00  140
 10  \w    -61.00  -3.00   0.50    8.00    --   16.91 -19.00-180.00  116
 11  \w    -69.00   3.00   0.50    8.00    --   16.91 -19.00-120.00  144
;
_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      -0.0014002000
_diffrn_orient_matrix_UB_12      0.0598780000
_diffrn_orient_matrix_UB_13      -0.0211342000
_diffrn_orient_matrix_UB_21      -0.0451913000
_diffrn_orient_matrix_UB_22      0.0116705000
_diffrn_orient_matrix_UB_23      0.0528656000
_diffrn_orient_matrix_UB_31      0.0641599000
_diffrn_orient_matrix_UB_32      -0.0093811000
_diffrn_orient_matrix_UB_33      0.0200872000
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.661
_diffrn_reflns_theta_min         2.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56517
_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    2.276
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.800
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0562P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5227
_reflns_number_total             6416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01897g2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7710883
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.747
_shelx_estimated_absorpt_t_max   0.747
_oxdiff_exptl_absorpt_empirical_full_min 0.629
_oxdiff_exptl_absorpt_empirical_full_max 1.665
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
016318139f290d04bb90afc7eb9416939100025d213
;
_diffrn_oxdiff_digest_hkl
;
0178e40006222c2306a996ad82649290eb8c3b
;
_shelx_res_checksum              7274