A direct reaction approach for the synthesis of zeolitic imidazolate frameworks: template and temperature mediated control on network topology and crystal size
Monica Lanchas; Daniel Vallejo-Sanchez; Garikoitz Beobide; Oscar Castillo; Andres T. Aguayo; Antonio Luque; Pascual Roman; Chem.Commun. 48 (2012) 9930–; doi:10.1039/c2cc34787c

data_7108388
_publ_section_title
;
 A direct reaction approach for the synthesis of zeolitic imidazolate
 frameworks: template and temperature mediated control on network topology
 and crystal size
;
_journal_name_full               Chem.Commun.
_journal_page_first              9930
_journal_paper_doi               10.1039/c2cc34787c
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H30 Co5 N20, 8 (H2 O), C6 H7 N'
_chemical_formula_structural     'C30 H30 Co5 N20, 8 (H2 O), C6 H7 N'
_chemical_formula_sum            'C36 H53 Co5 N21 O8'
_chemical_formula_weight         1202.64
_chemical_name_systematic
;
poly-[[dekakis(mu-imidazolato-KN:KN')pentacobalt(II)]-water-4-methylpyridine
(1/8/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.542(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3302(11)
_cell_length_b                   9.5623(5)
_cell_length_c                   24.6111(16)
_cell_measurement_reflns_used    21401
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.14
_cell_measurement_theta_min      2.52
_cell_volume                     5723.8(5)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_sigmaI/netI    0.1708
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21401
_diffrn_reflns_theta_full        67.14
_diffrn_reflns_theta_max         67.14
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.624
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.754
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                4296
_reflns_number_total             10225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34787c.txt
_cod_data_source_block           "'CoIMI4PIC'"
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7108388