The Heck reaction as a tool to expand polyoxovanadates towards thiol-sensitive organic-inorganic hybrid fluorescent switches.
Linnenberg, Oliver; Mayerl, Lisa; Monakhov, Kirill Yu; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14402–14407; doi:10.1039/c8dt02340a

data_7047294
_publ_section_title
;
 The Heck reaction as a tool to expand polyoxovanadates towards
 thiol-sensitive organic-inorganic hybrid fluorescent switches.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14402
_journal_page_last               14407
_journal_paper_doi               10.1039/c8dt02340a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C16 H36 N), Pd2 I6'
_chemical_formula_sum            'C32 H72 I6 N2 Pd2'
_chemical_formula_weight         1459.11
_chemical_name_systematic        (TBA)2[Pd2I6]
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2018-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5016(6)
_cell_length_b                   13.7745(5)
_cell_length_c                   23.8492(9)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.35
_cell_volume                     4664.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            69700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.006
_diffrn_reflns_theta_min         1.744
_exptl_absorpt_coefficient_mu    4.764
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1052 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.6613. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.273
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.139
_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     387
_refine_ls_number_reflns         13810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+12.5850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12091
_reflns_number_total             13810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02340a2.cif
_cod_data_source_block           pd2i6
_cod_depositor_comments
;
Adding full bibliography for 7047293--7047295.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(C16 H36 N), 2(Pd2 I6)'
_cod_original_formula_sum        'C64 H144 I12 N4 Pd4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2918.22
_cod_database_code               7047294
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              92536