#------------------------------------------------------------------------------
#$Date: 2021-09-06 12:10:31 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/86/7128656.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7128656
loop_
_publ_author_name
'Priebbenow, Daniel L.'
'Hua, Carol'
_publ_section_title
;
 Acyl silane directed Cp*Rh(III)-catalysed alkylation/annulation
 reactions.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7938
_journal_page_last               7941
_journal_paper_doi               10.1039/d1cc03051e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C15 H20 O2 Si'
_chemical_formula_sum            'C15 H20 O2 Si'
_chemical_formula_weight         260.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.140(3)
_cell_length_b                   7.0200(14)
_cell_length_c                   12.550(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1422.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33258
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.628
_diffrn_reflns_theta_min         2.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          4.250
_refine_ls_shift/su_mean         0.091
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1536P)²+0.2957P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1680
_reflns_number_total             1869
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc03051e2.cif
_cod_data_source_block           dp_18x
_cod_depositor_comments
'Adding full bibliography for 7128655--7128656.cif.'
_cod_database_code               7128656
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.969
_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. Others
 Fixed Sof: H8A(0.5) H8B(0.5) H11A(0.5) H11B(0.5) H11C(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.50103(3) 0.750000 0.19475(5) 0.0241(3) Uani 1 2 d S T P . .
O2 O 0.80209(10) 0.750000 0.60523(13) 0.0321(4) Uani 1 2 d S T P . .
O1 O 0.33885(10) 0.750000 0.31332(12) 0.0340(5) Uani 1 2 d S T P . .
C7 C 0.58661(13) 0.750000 0.51068(16) 0.0238(5) Uani 1 2 d S T P . .
C6 C 0.65163(13) 0.750000 0.58358(17) 0.0248(5) Uani 1 2 d S T P . .
H6 H 0.641506 0.750000 0.658146 0.030 Uiso 1 2 calc RS T P . .
C8 C 0.49574(12) 0.750000 0.53212(18) 0.0243(5) Uani 1 2 d S T P . .
H8A H 0.478910 0.864912 0.572408 0.029 Uiso 0.5 1 calc R . . . .
H8B H 0.478910 0.635088 0.572408 0.029 Uiso 0.5 1 calc R . . . .
C5 C 0.73209(13) 0.750000 0.54331(17) 0.0266(5) Uani 1 2 d S T P . .
C2 C 0.60001(13) 0.750000 0.39977(17) 0.0238(5) Uani 1 2 d S T P . .
C9 C 0.45888(13) 0.750000 0.42106(16) 0.0244(5) Uani 1 2 d S T P . .
C1 C 0.51905(15) 0.750000 0.34437(17) 0.0249(5) Uani 1 2 d S T P . .
C10 C 0.36862(14) 0.750000 0.40357(18) 0.0265(5) Uani 1 2 d S T P . .
C11 C 0.31365(14) 0.750000 0.50120(17) 0.0295(5) Uani 1 2 d S T P . .
H11A H 0.321165 0.869568 0.540331 0.044 Uiso 0.5 1 calc GR . . A -1
H11B H 0.328573 0.642572 0.547228 0.044 Uiso 0.5 1 calc GR . . A -1
H11C H 0.255611 0.737860 0.479294 0.044 Uiso 0.5 1 calc GR . . A -1
C4 C 0.74644(13) 0.750000 0.43360(18) 0.0282(5) Uani 1 2 d S T P . .
H4 H 0.801806 0.750000 0.407924 0.034 Uiso 1 2 calc RS T P . .
C3 C 0.68140(14) 0.750000 0.36143(16) 0.0261(5) Uani 1 2 d S T P . .
H3 H 0.691965 0.750000 0.286964 0.031 Uiso 1 2 calc RS T P . .
C14 C 0.60122(15) 0.750000 0.11966(18) 0.0312(5) Uani 1 2 d S T P . .
H14A H 0.635016 0.641487 0.142549 0.047 Uiso 0.5 1 calc GR . . B -1
H14B H 0.631128 0.868763 0.133970 0.047 Uiso 0.5 1 calc GR . . B -1
H14C H 0.589965 0.739750 0.043138 0.047 Uiso 0.5 1 calc GR . . B -1
C13 C 0.44792(10) 0.5254(3) 0.15409(13) 0.0337(4) Uani 1 1 d . . . . .
H13A H 0.433969 0.531761 0.078171 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.397104 0.509702 0.195902 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.484803 0.416905 0.166823 0.050 Uiso 1 1 calc GR . . . .
C12 C 0.79096(16) 0.750000 0.7179(2) 0.0376(6) Uani 1 2 d S T P . .
H12A H 0.844400 0.772060 0.752877 0.056 Uiso 0.5 1 calc GR . . C -1
H12B H 0.768663 0.626599 0.740504 0.056 Uiso 0.5 1 calc GR . . C -1
H12C H 0.752177 0.851341 0.737811 0.056 Uiso 0.5 1 calc GR . . C -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 Si1 C1 111.43(11) . . ?
C13 Si1 C1 109.92(6) . . ?
C13 Si1 C1 109.92(6) 7_575 . ?
C13 Si1 C14 105.02(7) 7_575 . ?
C13 Si1 C14 105.02(7) . . ?
C13 Si1 C13 115.35(11) 7_575 . ?
C5 O2 C12 117.28(18) . . ?
C6 C7 C8 128.52(19) . . ?
C6 C7 C2 122.2(2) . . ?
C2 C7 C8 109.23(19) . . ?
C5 C6 C7 117.65(19) . . ?
C7 C8 C9 102.72(17) . . ?
O2 C5 C6 124.2(2) . . ?
O2 C5 C4 114.97(19) . . ?
C6 C5 C4 120.81(19) . . ?
C7 C2 C1 109.19(19) . . ?
C3 C2 C7 118.95(19) . . ?
C3 C2 C1 131.87(19) . . ?
C1 C9 C8 111.62(18) . . ?
C1 C9 C10 126.7(2) . . ?
C10 C9 C8 121.69(18) . . ?
C2 C1 Si1 126.83(16) . . ?
C9 C1 Si1 125.93(18) . . ?
C9 C1 C2 107.24(18) . . ?
O1 C10 C9 121.6(2) . . ?
O1 C10 C11 121.1(2) . . ?
C9 C10 C11 117.33(19) . . ?
C3 C4 C5 121.2(2) . . ?
C4 C3 C2 119.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.900(2) . ?
Si1 C14 1.872(2) . ?
Si1 C13 1.8655(17) . ?
Si1 C13 1.8655(17) 7_575 ?
O2 C5 1.371(3) . ?
O2 C12 1.425(3) . ?
O1 C10 1.230(3) . ?
C7 C6 1.392(3) . ?
C7 C8 1.491(3) . ?
C7 C2 1.409(3) . ?
C6 C5 1.393(3) . ?
C8 C9 1.515(3) . ?
C5 C4 1.396(3) . ?
C2 C1 1.480(3) . ?
C2 C3 1.399(3) . ?
C9 C1 1.367(3) . ?
C9 C10 1.473(3) . ?
C10 C11 1.513(3) . ?
C4 C3 1.386(3) . ?
