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_7108496
_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            'C54 H41 Co2 N21 O13'
_chemical_formula_weight         1309.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           30
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2bc'
_symmetry_space_group_name_H-M   'P n c 2'
_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            2
_cell_length_a                   14.6913(3)
_cell_length_b                   27.1030(5)
_cell_length_c                   8.2799(1)
_cell_measurement_reflns_used    40031
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.64
_cell_volume                     3296.88(10)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'undulator KEK PF-NW2A'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38936
_diffrn_reflns_theta_full        32.37
_diffrn_reflns_theta_max         32.37
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9074
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.040(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         12312
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                9066
_reflns_number_total             12312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35078e.txt
_cod_data_source_block           TPHAP-Co-Therm-1
_cod_original_cell_volume        3296.9(1)
_cod_original_sg_symbol_H-M      Pnc2
_cod_database_code               7108496