Coordination polymers of alkali metal cyclosiloxazanides with one- and two-dimensional structures.
Jost, Maximilian; Richter, Roman-Malte; Balmer, Markus; Peters, Bertram; Dankert, Fabian; von Hänisch, Carsten; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5787–5790; doi:10.1039/d0dt01060j

data_1557842
_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         'C16 H48 K2 N2 O2 Si8, 2(C3.5 H3.5)'
_chemical_formula_sum            'C23 H55 K2 N2 O2 Si8'
_chemical_formula_weight         694.60
_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     iterative
_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                 100.1390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1709(8)
_cell_length_b                   21.2048(8)
_cell_length_c                   18.2698(7)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.23
_cell_volume                     8073.7(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0467
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55595
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.317
_diffrn_reflns_theta_min         2.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0649 before and 0.0523 after correction. The Ratio of minimum to maximum transmission is 0.9677. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+7.6417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6183
_reflns_number_total             7338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01060j2.cif
_cod_data_source_block           CvH-KNSi4O
_cod_depositor_comments
'Adding full bibliography for 1557842--1557846.cif.'
_cod_database_code               1557842
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.894
_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: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C24(H24)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C),
 C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C),
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C),
  C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              9334
_olex2_submission_special_instructions 'No special instructions were received'