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_7047293
_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
'(C24 H28 I2 O21 V6), 2(C16 H36 N), 1.5(C2 H3 N)'
_chemical_formula_sum            'C59 H102.5 I2 N3.5 O21 V6'
_chemical_formula_weight         1756.38
_chemical_name_systematic        (TBA)2_1
_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                 105.164(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.365(3)
_cell_length_b                   17.405(2)
_cell_length_c                   16.919(2)
_cell_measurement_reflns_used    5941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.34
_cell_volume                     7493.5(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART V5.631 (?, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_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            67274
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.646
_diffrn_reflns_theta_min         0.800
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1835 before and 0.1026 after correction. The Ratio of minimum to maximum transmission is 0.4855. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.444
_refine_diff_density_min         -2.475
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         15586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1490P)^2^+26.3270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10061
_reflns_number_total             15586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02340a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7047293--7047295.cif.'
_cod_original_cell_volume        7493.4(16)
_cod_original_formula_sum        'C59 H102.50 I2 N3.50 O21 V6'
_cod_database_code               7047293
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              51583