Reaction Progress Kinetics Analysis of 1,3-Disiloxanediols as Hydrogen-Bonding Catalysts.
Diemoz, Kayla M.; Hein, Jason E.; Wilson, Sean O.; Fettinger, James C.; Franz, Annaliese K.; The Journal of organic chemistry 82 (2017) 6738–6747; doi:10.1021/acs.joc.7b00875

data_4032729
_publ_section_title
;
 Reaction Progress Kinetics Analysis of 1,3-Disiloxanediols as
 Hydrogen-Bonding Catalysts.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6738
_journal_page_last               6747
_journal_paper_doi               10.1021/acs.joc.7b00875
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C40 H30 O3 Si2'
_chemical_formula_sum            'C40 H30 O3 Si2'
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_space_group_name_H-M_alt        'P 1'
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_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2016/6
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_cell_angle_beta                 102.3187(11)
_cell_angle_gamma                96.3662(12)
_cell_formula_units_Z            1
_cell_length_a                   7.2895(6)
_cell_length_b                   9.2340(8)
_cell_length_c                   11.6572(10)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.27
_cell_volume                     745.32(11)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex2 (2014.9-1) (Bruker, 2014)'
_computing_data_reduction        'SAINT (8.34a) (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.998
_diffrn_reflns_theta_min         1.828
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       Block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.49(10)
_refine_ls_extinction_coef       0.019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9305
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9110
_reflns_number_total             9305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00875_si_002.cif
_cod_data_source_block           JF2609FP1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4032729
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              55800
_shelx_hkl_checksum              11002