#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:53:38 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252808 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557843.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_1557843
loop_
_publ_author_name
'Jost, Maximilian'
'Richter, Roman-Malte'
'Balmer, Markus'
'Peters, Bertram'
'Dankert, Fabian'
'von Hänisch, Carsten'
_publ_section_title
;
 Coordination polymers of alkali metal cyclosiloxazanides with one- and
 two-dimensional structures.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5787
_journal_page_last               5790
_journal_paper_doi               10.1039/d0dt01060j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C8 H24 N O Rb Si4'
_chemical_formula_sum            'C8 H24 N O Rb Si4'
_chemical_formula_weight         348.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-30 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.493(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9604(2)
_cell_length_b                   16.9073(3)
_cell_length_c                   12.2222(3)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      67.998
_cell_measurement_theta_min      4.644
_cell_volume                     1745.49(7)
_computing_data_collection       'STOE X-AREA'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) and MS-Word'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Stadi-Cu
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15178
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         4.644
_exptl_absorpt_coefficient_mu    6.392
_exptl_absorpt_correction_T_max  45.09
_exptl_absorpt_correction_T_min  8.57
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'X-Area LANA 1.68.2.0 (STOE, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.016
_exptl_crystal_size_rad          0.112
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0406
_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/[σ²(Fo²)+(0.0897P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2894
_reflns_number_total             3170
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01060j2.cif
_cod_data_source_block           mj377
_cod_depositor_comments
'Adding full bibliography for 1557842--1557846.cif.'
_cod_database_code               1557843
_shelx_shelxl_version_number     2016/6
_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   0.905
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C2(H2A,
 H2B,H2C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Rb1 Rb 0.50196(3) 0.61011(2) 0.58650(2) 0.03548(15) Uani 1 1 d . . . . .
Si3 Si 0.30760(9) 0.57946(5) 0.26189(6) 0.0320(2) Uani 1 1 d . . . . .
Si1 Si 0.66582(9) 0.57734(5) 0.34038(6) 0.0319(2) Uani 1 1 d . . . . .
Si4 Si 0.30312(9) 0.67642(5) 0.12098(7) 0.0342(2) Uani 1 1 d . . . . .
Si2 Si 0.66119(9) 0.67682(5) 0.20231(7) 0.0347(2) Uani 1 1 d . . . . .
O1 O 0.4813(2) 0.71835(12) 0.15028(18) 0.0381(5) Uani 1 1 d . . . . .
N1 N 0.4884(3) 0.55923(15) 0.3539(2) 0.0333(5) Uani 1 1 d . . . . .
C6 C 0.1730(4) 0.61808(19) 0.3414(3) 0.0416(7) Uani 1 1 d . . . . .
H6A H 0.211175 0.669790 0.375508 0.062 Uiso 1 1 calc GR . . . .
H6B H 0.173275 0.580935 0.402979 0.062 Uiso 1 1 calc GR . . . .
H6C H 0.064980 0.623450 0.286575 0.062 Uiso 1 1 calc GR . . . .
C5 C 0.1954(4) 0.49093(19) 0.1802(3) 0.0433(7) Uani 1 1 d . . . . .
H5A H 0.096937 0.508709 0.121604 0.065 Uiso 1 1 calc GR . . . .
H5B H 0.170515 0.455013 0.234689 0.065 Uiso 1 1 calc GR . . . .
H5C H 0.260621 0.463184 0.142108 0.065 Uiso 1 1 calc GR . . . .
C4 C 0.7995(4) 0.76031(19) 0.2685(3) 0.0412(7) Uani 1 1 d . . . . .
H4A H 0.757151 0.791070 0.319454 0.062 Uiso 1 1 calc GR . . . .
H4B H 0.810193 0.794557 0.206822 0.062 Uiso 1 1 calc GR . . . .
H4C H 0.903480 0.738966 0.313751 0.062 Uiso 1 1 calc GR . . . .
C8 C 0.1651(4) 0.7595(2) 0.1216(3) 0.0436(7) Uani 1 1 d . . . . .
H8A H 0.058995 0.738251 0.109327 0.065 Uiso 1 1 calc GR . . . .
H8B H 0.161022 0.796787 0.059349 0.065 Uiso 1 1 calc GR . . . .
H8C H 0.203207 0.786804 0.196569 0.065 Uiso 1 1 calc GR . . . .
C2 C 0.8152(4) 0.6112(2) 0.4818(3) 0.0440(8) Uani 1 1 d . . . . .
H2A H 0.920189 0.614173 0.473588 0.066 Uiso 1 1 calc GR . . . .
H2B H 0.817908 0.573456 0.543304 0.066 Uiso 1 1 calc GR . . . .
H2C H 0.785123 0.663516 0.501962 0.066 Uiso 1 1 calc GR . . . .
C1 C 0.7615(4) 0.48742(19) 0.3001(3) 0.0436(7) Uani 1 1 d . . . . .
H1A H 0.686969 0.462405 0.231129 0.065 Uiso 1 1 calc GR . . . .
H1B H 0.790207 0.449734 0.364767 0.065 Uiso 1 1 calc GR . . . .
H1C H 0.856919 0.503483 0.283669 0.065 Uiso 1 1 calc GR . . . .
C7 C 0.2438(5) 0.6351(2) -0.0292(3) 0.0541(9) Uani 1 1 d . . . . .
H7A H 0.312433 0.590269 -0.030748 0.081 Uiso 1 1 calc GR . . . .
H7B H 0.254291 0.676091 -0.082855 0.081 Uiso 1 1 calc GR . . . .
H7C H 0.133533 0.617210 -0.052857 0.081 Uiso 1 1 calc GR . . . .
C3 C 0.7115(4) 0.6383(2) 0.0750(3) 0.0469(7) Uani 1 1 d . . . . .
H3A H 0.818989 0.616567 0.101957 0.070 Uiso 1 1 calc GR . . . .
H3B H 0.705451 0.681582 0.020343 0.070 Uiso 1 1 calc GR . . . .
H3C H 0.636239 0.596733 0.036271 0.070 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
N1 Rb1 O1 150.08(6) 3_666 4_576 ?
N1 Rb1 O1 123.00(6) . 4_576 ?
N1 Rb1 N1 86.72(6) . 3_666 ?
Si4 Si3 Rb1 146.34(3) . 3_666 ?
N1 Si3 Rb1 47.45(9) . 3_666 ?
N1 Si3 Si4 114.12(9) . . ?
N1 Si3 C6 111.39(14) . . ?
N1 Si3 C5 114.74(14) . . ?
C6 Si3 Rb1 107.36(10) . 3_666 ?
C6 Si3 Si4 105.92(10) . . ?
C5 Si3 Rb1 70.35(10) . 3_666 ?
C5 Si3 Si4 106.68(10) . . ?
C5 Si3 C6 103.03(15) . . ?
Si2 Si1 Rb1 148.99(3) . 3_666 ?
N1 Si1 Rb1 49.71(9) . 3_666 ?
N1 Si1 Si2 113.99(9) . . ?
N1 Si1 C2 111.72(14) . . ?
N1 Si1 C1 113.91(14) . . ?
C2 Si1 Rb1 104.88(10) . 3_666 ?
C2 Si1 Si2 105.97(11) . . ?
C2 Si1 C1 103.75(16) . . ?
C1 Si1 Rb1 68.53(10) . 3_666 ?
C1 Si1 Si2 106.68(10) . . ?
Si3 Si4 Rb1 141.26(3) . 4_575 ?
O1 Si4 Rb1 40.01(7) . 4_575 ?
O1 Si4 Si3 110.75(8) . . ?
O1 Si4 C8 105.41(13) . . ?
O1 Si4 C7 107.89(15) . . ?
C8 Si4 Rb1 69.59(10) . 4_575 ?
C8 Si4 Si3 111.52(10) . . ?
C7 Si4 Rb1 102.64(12) . 4_575 ?
C7 Si4 Si3 112.70(12) . . ?
C7 Si4 C8 108.23(17) . . ?
Si1 Si2 Rb1 144.88(3) . 4_575 ?
O1 Si2 Rb1 45.34(7) . 4_575 ?
O1 Si2 Si1 110.67(8) . . ?
O1 Si2 C4 105.17(13) . . ?
O1 Si2 C3 107.31(14) . . ?
C4 Si2 Rb1 64.94(10) . 4_575 ?
C4 Si2 Si1 112.01(10) . . ?
C3 Si2 Rb1 100.19(11) . 4_575 ?
C3 Si2 Si1 113.09(12) . . ?
C3 Si2 C4 108.18(15) . . ?
Si4 O1 Rb1 119.16(10) . 4_575 ?
Si4 O1 Si2 129.18(13) . . ?
Si2 O1 Rb1 111.44(9) . 4_575 ?
Rb1 N1 Rb1 93.28(6) . 3_666 ?
Si3 N1 Rb1 107.87(11) . 3_666 ?
Si3 N1 Rb1 108.04(11) . . ?
Si3 N1 Si1 129.27(14) . . ?
Si1 N1 Rb1 104.52(11) . 3_666 ?
Si1 N1 Rb1 107.91(11) . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Rb1 C5 H5A 166.1 3_666 . ?
Rb1 C5 H5B 57.0 3_666 . ?
Rb1 C5 H5C 75.0 3_666 . ?
Si3 C5 Rb1 80.34(10) . 3_666 ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Rb1 C4 H4A 72.8 4_575 . ?
Rb1 C4 H4B 53.6 4_575 . ?
Rb1 C4 H4C 160.7 4_575 . ?
Si2 C4 Rb1 86.84(11) . 4_575 ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Rb1 C1 H1A 77.5 3_666 . ?
Rb1 C1 H1B 53.7 3_666 . ?
Rb1 C1 H1C 163.0 3_666 . ?
Si1 C1 Rb1 81.51(10) . 3_666 ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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
Rb1 O1 3.025(2) 4_576 ?
Rb1 N1 2.933(2) . ?
Rb1 N1 2.948(2) 3_666 ?
Si3 Si4 2.3683(11) . ?
Si3 N1 1.671(2) . ?
Si3 C6 1.899(3) . ?
Si3 C5 1.891(3) . ?
Si1 Si2 2.3732(10) . ?
Si1 N1 1.680(2) . ?
Si1 C2 1.888(4) . ?
Si1 C1 1.889(3) . ?
Si4 O1 1.673(2) . ?
Si4 C8 1.873(3) . ?
Si4 C7 1.868(3) . ?
Si2 O1 1.677(2) . ?
Si2 C4 1.875(3) . ?
Si2 C3 1.874(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
