Pore-controlled formation of 0D metal complexes in anionic 3D metal‒organic frameworks
Zhang, Muwei; Bosch, Mathieu; Zhou, Hong-Cai; CrystEngComm 17 (2015) 996–; doi:10.1039/C4CE02261K

data_7219037
_publ_section_title
;
 Pore-controlled formation of 0D metal complexes in anionic 3D
 metal--organic frameworks
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              996
_journal_paper_doi               10.1039/C4CE02261K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C56 H32 Cd3 O16 Si2, C16 H40 Cd N4 O6, 2(C4 H9 N O)'
_chemical_formula_sum            'C80 H90 Cd4 N6 O24 Si2'
_chemical_formula_weight         2025.36
_chemical_name_systematic        'PCN-514-DMA complex'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4779)
;
_audit_update_record
;
2014-11-11 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                115.6630(10)
_cell_angle_beta                 113.6270(10)
_cell_angle_gamma                97.603(2)
_cell_formula_units_Z            1
_cell_length_a                   14.0970(19)
_cell_length_b                   14.2015(19)
_cell_length_c                   14.2649(19)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.63
_cell_volume                     2190.6(5)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24914
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0615 before and 0.0386 after correction.
The Ratio of minimum to maximum transmission is 0.8654.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_recrystallization_method 'Solvothermal MOF Synthesis'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.8126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                8687
_reflns_number_total             9495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02261k2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7219037--7219199.cif.'
_cod_database_code               7219037
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C3(H3), C14(H14), C7(H7), C27(H27), C25(H25),
 C4(H4), C28(H28), C20(H20), C18(H18), C17(H17), C24(H24), C6(H6), C21(H21)
2.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C29(H29A,H29B,H29C), C32(H32A,
 H32B,H32C), C31(H31A,H31B,H31C)
;
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'