Interpenetrated Frameworks with Anisotropic Pore Structures from a Tetrahedral Pyridine Ligand
Geyer, Florian L.; Rominger, Frank; Vogtland, Maximilian; Bunz, Uwe H. F.; Crystal Growth & Design 15 (2015) 3539–; doi:10.1021/acs.cgd.5b00719

data_4513237
_publ_section_title
;
 Interpenetrated Frameworks with Anisotropic Pore Structures from a
 Tetrahedral Pyridine Ligand
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3539
_journal_paper_doi               10.1021/acs.cgd.5b00719
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C52 H32 N4 Si'
_chemical_formula_weight         740.90
_chemical_name_common            '1 (second modification) in manuscript'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.3062(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0422(6)
_cell_length_b                   29.432(2)
_cell_length_c                   15.6532(11)
_cell_measurement_reflns_used    7644
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.83
_cell_measurement_theta_min      2.32
_cell_volume                     4036.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35013
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.871
_diffrn_reflns_theta_min         1.343
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.8405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
; 
 Flack x determined using 3343 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         13731
_refine_ls_number_restraints     901
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0533P)^2^+1.2139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                9542
_reflns_number_total             13731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00719_si_002.cif
_cod_data_source_block           fge21
_cod_depositor_comments
'Adding full bibliography for 4513232--4513239.cif.'
_cod_database_code               4513237
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014-3
_shelx_res_checksum              68140
_shelx_hkl_checksum              88866