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_7716394
_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 Si, C8 H20 N'
_chemical_formula_sum            'C34 H33 F12 N O2 Si'
_chemical_formula_weight         743.70
_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             2021-08-06
_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                 95.844(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0531(2)
_cell_length_b                   16.2521(3)
_cell_length_c                   18.3816(3)
_cell_measurement_reflns_used    21503
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.3570
_cell_measurement_theta_min      2.0690
_cell_volume                     3284.84(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -105.26  94.54   1.80   30.00 -23.04  -4.70  73.83    --   111
  2  \w    -23.03 140.77   1.80   30.00    --   -4.70  73.83 -25.77   91
  3  \w    -23.03 140.77   1.80   30.00    --   -4.70  73.83  46.23   91
  4  \w    -23.03 140.77   1.80   30.00    --   -4.70  73.83 -97.77   91
  5  \w    -23.03 140.77   1.80   30.00    --   -4.70  73.83-169.77   91
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0498894000
_diffrn_orient_matrix_UB_12      -0.0061556000
_diffrn_orient_matrix_UB_13      -0.0207883000
_diffrn_orient_matrix_UB_21      0.0398805000
_diffrn_orient_matrix_UB_22      -0.0020745000
_diffrn_orient_matrix_UB_23      0.0327167000
_diffrn_orient_matrix_UB_31      -0.0090285000
_diffrn_orient_matrix_UB_32      -0.0431627000
_diffrn_orient_matrix_UB_33      0.0013695000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            102131
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.581
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (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    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0214P)^2^+3.0091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7201
_reflns_number_total             7533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01688b2.cif
_cod_data_source_block           20210805_siw01018
_cod_depositor_comments
'Adding full bibliography for 7716394--7716396.cif.'
_cod_database_code               7716394
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 99.87
_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:
 C31(H31A,H31B), C33(H33A,H33B), C27(H27A,H27B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C26(H26), C15(H15), C25(H25), C14(H14), C12(H12), C24(H24),
 C23(H23), C13(H13), C6(H6), C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              11169
_shelx_hkl_checksum              66635
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.646