Metal–organic frameworks with oxazoline-containing tripodal ligand: structure changes via reaction medium and metal-to-ligand ratio
Huang, Yong-Qing; Shen, Zhong-Liang; Zhou, Xia-Ying; Okamura, Taka-aki; Su, Zhi; Fan, Jian; Sun, Wei-Yin; Yu, Jin-Quan; Ueyama, Norikazu; CrystEngComm 12 (2010) 4328–; doi:10.1039/c002874f

data_7212651
_publ_section_title
;
 Metal--organic frameworks with oxazoline-containing tripodal ligand:
 structure changes via reaction medium and metal-to-ligand ratio
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4328
_journal_paper_doi               10.1039/c002874f
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C36 H39 Cl3 Cu3 N9 O18'
_chemical_formula_weight         1182.73
_chemical_name_systematic
;
[Cu3(OX1)2(MeCN)3](ClO4)3
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   23.752(2)
_cell_length_b                   23.752
_cell_length_c                   14.2281(12)
_cell_measurement_reflns_used    1771
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.97
_cell_volume                     6951.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_sigmaI/netI    0.1231
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12129
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                1628
_reflns_number_total             2856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002874f.txt
_cod_data_source_block           2
_cod_original_cell_volume        6951.3(8)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7212651