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_7212652
_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_moiety         'C31.50 H36.75 Cl2 Cu2 N6.75 O12.25 '
_chemical_formula_sum            'C31.5 H36.75 Cl2 Cu2 N6.75 O12.25'
_chemical_formula_weight         903.91
_chemical_name_systematic
;
[Cu2Cl(OX1)2](ClO4)-9/4(H2O)-3/4(CH3CN)
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      59
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Tue Apr 10 16:17:47 2007'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.988(11)
_cell_length_b                   25.016(12)
_cell_length_c                   13.119(5)
_cell_measurement_reflns_used    14535
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     7544(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1706
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            55253
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            greenish-yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.2272
_refine_ls_R_factor_gt           0.1452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3738
_refine_ls_wR_factor_ref         0.4192
_reflns_number_gt                3623
_reflns_number_total             6987
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c002874f.txt
_cod_data_source_block           3
_cod_original_cell_volume        7545(6)
_cod_original_sg_symbol_H-M      'P m m n'
_cod_original_formula_sum        'C31.50 H36.75 Cl2 Cu2 N6.75 O12.25'
_cod_database_code               7212652