Synthesis, structure, and alkynylation reactivity of alkynyl-silicate, -germanate, and -stannate.
Iwabuchi, Shuta; Morofuji, Tatsuya; Kano, Naokazu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10829–10833; doi:10.1039/d4dt01688b

data_7716395
_publ_section_title
;
 Synthesis, structure, and alkynylation reactivity of alkynyl-silicate,
 -germanate, and -stannate.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10829
_journal_page_last               10833
_journal_paper_doi               10.1039/d4dt01688b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H13 F12 O2 Sn, C8 H20 N'
_chemical_formula_sum            'C34 H33 F12 N O2 Sn'
_chemical_formula_weight         834.30
_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     dual
_audit_creation_date             2021-12-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.334(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2117(4)
_cell_length_b                   16.2237(7)
_cell_length_c                   18.2776(8)
_cell_measurement_reflns_used    12553
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.5660
_cell_measurement_theta_min      2.0360
_cell_volume                     3304.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Rigaku HyPix-3000 area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_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    -44.00 110.00   0.50   22.05    --   20.00  54.00 150.00  308
  2  \w    -67.00 -21.00   0.50   22.05    --   20.00  54.00 -90.00   92
  3  \w     -3.00  74.00   0.50   22.05    --   20.00  54.00 -90.00  154
  4  \w    -72.00 -33.00   0.50   22.05    --   20.00  54.00 120.00   78
  5  \w     -9.00  16.00   0.50   22.05    --   20.00  54.00 120.00   50
  6  \w     44.00 108.00   0.50   22.05    --   20.00  54.00 120.00  128
  7  \w    -73.00 -18.00   0.50   22.05    --   20.00  54.00 -30.00  110
  8  \w     16.00  41.00   0.50   22.05    --   20.00  54.00 -30.00   50
  9  \w    -71.00 -46.00   0.50   22.05    --   20.00  54.00-150.00   50
 10  \w     22.00  47.00   0.50   22.05    --   20.00  54.00-150.00   50
 11  \w     16.00  85.00   0.50   22.05    --   20.00  54.00-120.00  138
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0230143000
_diffrn_orient_matrix_UB_12      -0.0053347000
_diffrn_orient_matrix_UB_13      0.0343419000
_diffrn_orient_matrix_UB_21      0.0387965000
_diffrn_orient_matrix_UB_22      -0.0341704000
_diffrn_orient_matrix_UB_23      0.0078537000
_diffrn_orient_matrix_UB_31      0.0448595000
_diffrn_orient_matrix_UB_32      0.0267375000
_diffrn_orient_matrix_UB_33      0.0168895000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35507
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.787
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00042(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         9946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0230P)^2^+1.4850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7299
_reflns_number_total             9946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01688b2.cif
_cod_data_source_block           20211218iwabuchi1_auto
_cod_depositor_comments
'Adding full bibliography for 7716394--7716396.cif.'
_cod_database_code               7716395
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H33 F12 N O2 Sn'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C35(H35A,H35B), C41(H41A,H41B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C22(H22), C44(H44), C4(H4), C47(H47), C48(H48), C21(H21),
 C46(H46), C3(H3), C45(H45), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C)
;
_shelx_res_checksum              45113
_shelx_hkl_checksum              36085
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.024
_oxdiff_exptl_absorpt_empirical_full_min 0.963