Homoconjugated Acids as Low Cyclosiloxane-Producing Silanol Polycondensation Catalysts
Roberts, John M.; Belowich, Matthew E.; Peterson, Thomas H.; Bellinger, Edward; Syverud, Karin; Laitar, David S.; Sidle, Tobias; ACS Omega 5 (2020) 24954–24963; doi:10.1021/acsomega.0c03883

data_4518063
_publ_section_title
;
 Homoconjugated Acids as Low Cyclosiloxane-Producing Silanol
 Polycondensation Catalysts
;
_journal_issue                   38
_journal_name_full               'ACS Omega'
_journal_page_first              24954
_journal_page_last               24963
_journal_paper_doi               10.1021/acsomega.0c03883
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         '2(C7 H4.5 Br O2), C5 H14 N3'
_chemical_formula_sum            'C19 H23 Br2 N3 O4'
_chemical_formula_weight         517.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2937(9)
_cell_angle_gamma                90
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_cell_length_a                   9.7284(6)
_cell_length_b                   10.1848(6)
_cell_length_c                   21.6633(13)
_cell_measurement_reflns_used    756
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      4.1867
_cell_volume                     2137.3(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.631
_diffrn_reflns_theta_min         1.888
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.822
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+1.4016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2983
_reflns_number_total             3280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03883_si_002.cif
_cod_data_source_block           2017_07_19_17_bn6058_roberts_0
_cod_depositor_comments          'Adding full bibliography for 4518063.cif.'
_cod_database_code               4518063
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.439
_shelx_estimated_absorpt_t_min   0.379
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
3.b Idealised Me refined as rotating group:
 C8(HA,HB,HC), C9(HD,HE,HF)
;
_shelx_res_checksum              12241
_shelx_hkl_checksum              92929
_olex2_date_sample_data_collection 2017-07-19
_olex2_date_sample_submission    2017-07-19
_olex2_submission_special_instructions 'No special instructions were received'