Crystal surface mediated structure transformation of a kinetic framework composed of multi-interactive ligand TPHAP and Co(II)
Yumi Yakiyama; Akira Ueda; Yasushi Morita; Masaki Kawano; Chem.Commun. 48 (2012) 10651–; doi:10.1039/c2cc35078e

data_7108495
_publ_section_title
;
 Crystal surface mediated structure transformation of a kinetic framework
 composed of multi-interactive ligand TPHAP and Co(II)
;
_journal_name_full               Chem.Commun.
_journal_page_first              10651
_journal_paper_doi               10.1039/c2cc35078e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C57.28 H35 Co N19.31 O13.68'
_chemical_formula_weight         1271.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.0224(5)
_cell_length_b                   8.4172(1)
_cell_length_c                   27.4938(4)
_cell_measurement_reflns_used    57846
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.69
_cell_volume                     6716.39(17)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku Crystal Clear'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  Si
_diffrn_radiation_source         'undulator KEK PF-NW2A'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            111153
_diffrn_reflns_theta_full        29.90
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9433
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2601
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.261(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         20585
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                13339
_reflns_number_total             20585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35078e.txt
_cod_data_source_block           TPHAP-Cokin
_cod_original_cell_volume        6716.4(2)
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7108495