Unprecedented solvent induced inter-conversion between monomeric and dimeric silylene-zinc iodide adducts
Yadav, Sandeep; Sangtani, Ekta; Dhawan, Diksha; Gonnade, Rajesh G.; Ghosh, Debashree; Sen, Sakya Singha; Dalton Trans.  (2017) –; doi:10.1039/C7DT01823A

data_7043913
_publ_section_title
;
 Unprecedented solvent induced inter-conversion between monomeric and
 dimeric silylene-zinc iodide adducts
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01823A
_journal_year                    2017
_chemical_formula_moiety         'C25 H49 I2 N3 O1 Si3 Zn, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C27 H53 I2 N3 O2 Si3 Zn'
_chemical_formula_weight         855.16
_chemical_melting_point          406
_chemical_name_systematic        1
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-18 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                88.975(4)
_cell_angle_beta                 86.600(4)
_cell_angle_gamma                70.447(4)
_cell_formula_units_Z            2
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_cell_length_b                   9.851(2)
_cell_length_c                   19.935(5)
_cell_measurement_reflns_used    6076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.38
_cell_volume                     1815.0(7)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon 100 Area Detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1626
_diffrn_reflns_av_unetI/netI     0.1648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30496
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Incoatech I\mS HB'
_exptl_absorpt_coefficient_mu    2.503
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0265P)^2^+7.0694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4203
_reflns_number_total             7897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01823a2.cif
_cod_data_source_block           Q1_a
_cod_original_cell_volume        1814.9(8)
_cod_database_code               7043913
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.648
_shelx_res_checksum              43408