Stereochemically Distinct Cyclotetrasiloxanes Containing 3-Pyridyl Moieties and Their Functional Coordination Polymers.
Deshmukh, Mahesh S.; Vijayakanth, Thangavel; Boomishankar, Ramamoorthy; Inorganic chemistry 55 (2016) 3098–3104; doi:10.1021/acs.inorgchem.6b00001

data_4347311
_publ_section_title
;
 Stereochemically Distinct Cyclotetrasiloxanes Containing 3-Pyridyl
 Moieties and Their Functional Coordination Polymers.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3098
_journal_page_last               3104
_journal_paper_doi               10.1021/acs.inorgchem.6b00001
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C32 H44 Cu4 I4 N4 O4 Si4'
_chemical_formula_weight         1422.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 109.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.29(3)
_cell_length_b                   11.09(2)
_cell_length_c                   16.96(3)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.64
_cell_volume                     2882(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Smart Apex Duo'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  1.1990
_diffrn_reflns_av_unetI/netI     0.8960
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.571
_diffrn_reflns_theta_min         1.837
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       square
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.938
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.304
_refine_ls_extinction_coef       0.0012(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.5163
_refine_ls_R_factor_gt           0.1796
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4207
_refine_ls_wR_factor_ref         0.5447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1304
_reflns_number_total             7227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00001_si_004.cif
_cod_data_source_block           Compound_3
_cod_original_cell_volume        2880(9)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4347311
_shelxl_version_number           2014/6
_shelx_res_checksum              15708
_shelx_hkl_checksum              17230