#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:46:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180053 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/47/7034735.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_7034735
loop_
_publ_author_name
'Evans, Lloyd T. J.'
'Farnaby, Joy H.'
'Coles, Martyn P.'
'Cloke, F Geoffrey N'
'Hitchcock, Peter B.'
_publ_section_title
;
 Group 4 metal compounds incorporating the amide ligand,
 [N(SiMe2{C6H4-2-OMe})2](.).
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8950
_journal_page_last               8958
_journal_paper_doi               10.1039/c5dt00684h
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H52 K2 N2 O4 Si4'
_chemical_formula_sum            'C36 H52 K2 N2 O4 Si4'
_chemical_formula_weight         767.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-06-17T11:13:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-01-19 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.406(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8637(3)
_cell_length_b                   8.4515(2)
_cell_length_c                   19.6313(4)
_cell_measurement_reflns_used    19281
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2111.34(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.594371E-1
_diffrn_orient_matrix_UB_12      -0.556264E-1
_diffrn_orient_matrix_UB_13      0.288633E-1
_diffrn_orient_matrix_UB_21      0.300748E-1
_diffrn_orient_matrix_UB_22      0.104353
_diffrn_orient_matrix_UB_23      0.168966E-1
_diffrn_orient_matrix_UB_31      -0.416885E-1
_diffrn_orient_matrix_UB_32      -0.40267E-2
_diffrn_orient_matrix_UB_33      0.391518E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20378
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+0.8149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                3609
_reflns_number_total             4139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00684h2.cif
_cod_data_source_block           (2)-jun1605
_cod_depositor_comments
'Adding full bibliography for 7034734--7034738.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7034735
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
K K 0.60080(3) 0.64234(4) 0.529085(19) 0.02965(11) Uani 1 1 d
Si1 Si 0.65213(3) 0.23118(5) 0.57224(2) 0.02428(12) Uani 1 1 d
Si2 Si 0.68169(3) 0.30736(5) 0.42858(2) 0.02439(12) Uani 1 1 d
O1 O 0.72461(11) 0.54204(16) 0.64726(6) 0.0464(3) Uani 1 1 d
O2 O 0.78567(10) 0.62076(16) 0.47441(7) 0.0433(3) Uani 1 1 d
N N 0.62047(10) 0.32819(15) 0.49800(6) 0.0236(3) Uani 1 1 d
C1 C 0.65601(17) 0.0086(2) 0.56249(12) 0.0405(4) Uani 1 1 d
H1B H 0.5855(19) -0.026(3) 0.5415(12) 0.064(7) Uiso 1 1 d
H1C H 0.6751(17) -0.043(3) 0.6071(11) 0.055(6) Uiso 1 1 d
H1A H 0.7003(18) -0.019(3) 0.5309(11) 0.057(6) Uiso 1 1 d
C2 C 0.55341(15) 0.2634(3) 0.63216(10) 0.0397(4) Uani 1 1 d
H2B H 0.575(2) 0.210(3) 0.6750(14) 0.078(8) Uiso 1 1 d
H2C H 0.4885(19) 0.221(3) 0.6145(11) 0.057(6) Uiso 1 1 d
H2A H 0.5442(19) 0.368(3) 0.6399(12) 0.067(8) Uiso 1 1 d
C3 C 0.78624(13) 0.2875(2) 0.62100(8) 0.0314(4) Uani 1 1 d
C4 C 0.80830(14) 0.4350(2) 0.65103(8) 0.0388(4) Uani 1 1 d
C5 C 0.90882(18) 0.4778(3) 0.68232(10) 0.0563(6) Uani 1 1 d
H5 H 0.9146(18) 0.580(3) 0.7015(12) 0.062(7) Uiso 1 1 d
C6 C 0.98993(17) 0.3696(4) 0.68393(11) 0.0637(7) Uani 1 1 d
H6 H 1.058(2) 0.397(3) 0.7052(13) 0.077(8) Uiso 1 1 d
C7 C 0.97155(16) 0.2224(4) 0.65667(10) 0.0555(6) Uani 1 1 d
H7 H 1.028(2) 0.146(3) 0.6579(12) 0.067(7) Uiso 1 1 d
C8 C 0.87165(14) 0.1828(3) 0.62577(9) 0.0420(5) Uani 1 1 d
H8 H 0.8609(16) 0.077(3) 0.6077(11) 0.052(6) Uiso 1 1 d
C9 C 0.7218(4) 0.6401(5) 0.70492(15) 0.0898(12) Uani 1 1 d
H9C H 0.771(4) 0.733(7) 0.709(3) 0.22(3) Uiso 1 1 d
H9B H 0.741(3) 0.584(4) 0.7443(18) 0.109(11) Uiso 1 1 d
H9A H 0.658(2) 0.687(3) 0.7001(14) 0.076(8) Uiso 1 1 d
C10 C 0.61197(18) 0.1621(2) 0.36550(10) 0.0409(4) Uani 1 1 d
H10B H 0.5418(19) 0.190(3) 0.3503(11) 0.051(6) Uiso 1 1 d
H10C H 0.6111(18) 0.060(3) 0.3891(12) 0.065(7) Uiso 1 1 d
H10A H 0.6435(18) 0.144(3) 0.3261(12) 0.058(7) Uiso 1 1 d
C11 C 0.82275(15) 0.2382(3) 0.44406(11) 0.0389(4) Uani 1 1 d
H11C H 0.8286(17) 0.131(3) 0.4656(11) 0.055(6) Uiso 1 1 d
H11A H 0.8501(19) 0.237(3) 0.4017(13) 0.067(7) Uiso 1 1 d
H11B H 0.8636(19) 0.304(3) 0.4762(12) 0.062(7) Uiso 1 1 d
C12 C 0.68782(12) 0.4982(2) 0.37785(8) 0.0292(4) Uani 1 1 d
C13 C 0.74390(13) 0.6310(2) 0.40524(9) 0.0349(4) Uani 1 1 d
C14 C 0.75336(16) 0.7674(2) 0.36670(12) 0.0465(5) Uani 1 1 d
H14 H 0.7903(16) 0.854(2) 0.3887(10) 0.045(6) Uiso 1 1 d
C15 C 0.70729(17) 0.7722(3) 0.29866(12) 0.0518(6) Uani 1 1 d
H15 H 0.7141(19) 0.867(3) 0.2730(12) 0.068(7) Uiso 1 1 d
C16 C 0.65196(18) 0.6449(3) 0.26944(11) 0.0495(6) Uani 1 1 d
H16 H 0.6198(17) 0.650(3) 0.2227(12) 0.057(6) Uiso 1 1 d
C17 C 0.64206(15) 0.5102(2) 0.30850(9) 0.0375(4) Uani 1 1 d
H17 H 0.6027(14) 0.422(2) 0.2879(9) 0.036(5) Uiso 1 1 d
C18 C 0.88260(19) 0.6986(4) 0.49657(16) 0.0612(6) Uani 1 1 d
H18A H 0.933(2) 0.676(3) 0.4684(15) 0.085(9) Uiso 1 1 d
H18B H 0.870(3) 0.816(4) 0.4962(17) 0.109(11) Uiso 1 1 d
H18C H 0.910(2) 0.661(3) 0.5406(14) 0.063(7) Uiso 1 1 d
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
N K O1 80.12(4) . .
N K O2 74.71(4) . .
O1 K O2 83.21(4) . .
N K N 99.57(3) . 3_666
O1 K N 128.95(4) . 3_666
O2 K N 146.60(4) . 3_666
N K C1 161.81(5) . 1_565
O1 K C1 92.36(5) . 1_565
O2 K C1 88.04(5) . 1_565
N K C1 98.02(5) 3_666 1_565
N Si1 C2 112.06(8) . .
N Si1 C1 113.99(8) . .
C2 Si1 C1 103.80(10) . .
N Si1 C3 113.76(7) . .
C2 Si1 C3 107.17(9) . .
C1 Si1 C3 105.28(9) . .
N Si2 C10 111.62(8) . .
N Si2 C11 117.08(8) . .
C10 Si2 C11 105.01(10) . .
N Si2 C12 113.32(7) . .
C10 Si2 C12 105.17(9) . .
C11 Si2 C12 103.55(8) . .
C4 O1 C9 116.61(18) . .
C4 O1 K 126.16(9) . .
C9 O1 K 114.67(16) . .
C13 O2 C18 117.88(17) . .
C13 O2 K 98.30(9) . .
C18 O2 K 128.25(15) . .
Si1 N Si2 124.96(8) . .
Si1 N K 107.43(6) . .
Si2 N K 110.56(6) . .
Si1 N K 108.52(6) . 3_666
Si2 N K 115.78(6) . 3_666
K N K 80.43(3) . 3_666
Si1 C1 K 165.33(10) . 1_545
Si1 C1 H1B 107.5(14) . .
K C1 H1B 57.8(14) 1_545 .
Si1 C1 H1C 111.0(13) . .
K C1 H1C 76.9(13) 1_545 .
H1B C1 H1C 109.8(19) . .
Si1 C1 H1A 110.1(14) . .
K C1 H1A 76.2(14) 1_545 .
H1B C1 H1A 105.2(18) . .
H1C C1 H1A 112.8(19) . .
Si1 C2 H2B 110.4(15) . .
Si1 C2 H2C 111.4(14) . .
H2B C2 H2C 106(2) . .
Si1 C2 H2A 111.3(16) . .
H2B C2 H2A 110(2) . .
H2C C2 H2A 108(2) . .
C4 C3 C8 115.33(17) . .
C4 C3 Si1 123.38(13) . .
C8 C3 Si1 121.21(15) . .
C3 C4 C5 122.52(19) . .
C3 C4 O1 116.71(15) . .
C5 C4 O1 120.75(19) . .
C6 C5 C4 119.0(2) . .
C6 C5 H5 125.6(15) . .
C4 C5 H5 115.4(15) . .
C7 C6 C5 120.5(2) . .
C7 C6 H6 119.7(16) . .
C5 C6 H6 119.8(17) . .
C6 C7 C8 119.5(2) . .
C6 C7 H7 120.6(15) . .
C8 C7 H7 119.9(15) . .
C7 C8 C3 123.1(2) . .
C7 C8 H8 117.5(13) . .
C3 C8 H8 119.4(13) . .
O1 C9 H9C 115(3) . .
O1 C9 H9B 110(2) . .
H9C C9 H9B 105(4) . .
O1 C9 H9A 107.7(18) . .
H9C C9 H9A 103(4) . .
H9B C9 H9A 117(3) . .
Si2 C10 H10B 113.1(13) . .
Si2 C10 H10C 107.5(13) . .
H10B C10 H10C 107.1(19) . .
Si2 C10 H10A 115.3(14) . .
H10B C10 H10A 106.8(19) . .
H10C C10 H10A 106.6(19) . .
Si2 C11 H11C 111.1(13) . .
Si2 C11 H11A 109.4(14) . .
H11C C11 H11A 110.3(19) . .
Si2 C11 H11B 110.8(14) . .
H11C C11 H11B 104.5(19) . .
H11A C11 H11B 111(2) . .
C13 C12 C17 115.74(16) . .
C13 C12 Si2 122.50(12) . .
C17 C12 Si2 121.61(14) . .
O2 C13 C14 122.04(18) . .
O2 C13 C12 115.49(15) . .
C14 C13 C12 122.40(18) . .
C15 C14 C13 119.3(2) . .
C15 C14 H14 122.5(13) . .
C13 C14 H14 118.2(13) . .
C16 C15 C14 120.41(19) . .
C16 C15 H15 121.3(15) . .
C14 C15 H15 118.3(15) . .
C15 C16 C17 119.8(2) . .
C15 C16 H16 119.8(14) . .
C17 C16 H16 120.5(14) . .
C16 C17 C12 122.3(2) . .
C16 C17 H17 119.4(11) . .
C12 C17 H17 118.3(11) . .
O2 C18 H18A 111.9(18) . .
O2 C18 H18B 109.0(19) . .
H18A C18 H18B 109(3) . .
O2 C18 H18C 108.8(15) . .
H18A C18 H18C 106(2) . .
H18B C18 H18C 112(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K N 2.7442(13) .
K O1 2.7490(13) .
K O2 2.7546(13) .
K N 2.8291(13) 3_666
K C1 3.222(2) 1_565
Si1 N 1.6699(13) .
Si1 C2 1.8728(18) .
Si1 C1 1.8925(19) .
Si1 C3 1.9069(17) .
Si2 C10 1.8765(19) .
Si2 C11 1.8883(19) .
Si2 C12 1.9037(17) .
O1 C4 1.400(2) .
O1 C9 1.408(3) .
O2 C13 1.388(2) .
O2 C18 1.421(2) .
C1 H1B 0.98(2) .
C1 H1C 0.98(2) .
C1 H1A 0.93(2) .
C2 H2B 0.96(3) .
C2 H2C 0.93(2) .
C2 H2A 0.91(3) .
C3 C4 1.390(3) .
C3 C8 1.403(3) .
C4 C5 1.396(3) .
C5 C6 1.384(4) .
C5 H5 0.94(3) .
C6 C7 1.361(4) .
C6 H6 0.94(3) .
C7 C8 1.380(3) .
C7 H7 0.97(3) .
C8 H8 0.97(2) .
C9 H9C 1.01(6) .
C9 H9B 0.91(3) .
C9 H9A 0.91(3) .
C10 H10B 0.94(2) .
C10 H10C 0.98(3) .
C10 H10A 0.94(2) .
C11 H11C 1.00(2) .
C11 H11A 0.95(3) .
C11 H11B 0.94(3) .
C12 C13 1.398(2) .
C12 C17 1.406(2) .
C13 C14 1.394(3) .
C14 C15 1.380(3) .
C14 H14 0.94(2) .
C15 C16 1.369(3) .
C15 H15 0.96(2) .
C16 C17 1.389(3) .
C16 H16 0.95(2) .
C17 H17 0.96(2) .
C18 H18A 0.93(3) .
C18 H18B 1.00(4) .
C18 H18C 0.94(3) .
