A three-dimensional structure built of paddle-wheel and triazolate-dinuclear metal clusters: synthesis, deformation and reformation of paddle-wheel unit in the single-crystal-to-single-crystal transformation
Yang, Feilong; Zheng, Qingshu; Chen, Zhenxia; Ling, Yun; Liu, Xiaofeng; Weng, Linhong; Zhou, Yaming; CrystEngComm 15 (2013) 7031–; doi:10.1039/c3ce40855h

data_7210390
_publ_section_title
;
 A three-dimensional structure built of paddle-wheel and
 triazolate-dinuclear metal clusters: synthesis, deformation and
 reformation of paddle-wheel unit in the single-crystal-to-single-crystal
 transformation
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              7031
_journal_paper_doi               10.1039/c3ce40855h
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C18 H11 N5 O8.5 Zn2, (C2 H8 N), (H2 O)'
_chemical_formula_sum            'C20 H21 N6 O9.5 Zn2'
_chemical_formula_weight         628.17
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.466(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.230(4)
_cell_length_b                   21.274(10)
_cell_length_c                   14.195(7)
_cell_measurement_reflns_used    922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.352
_cell_measurement_theta_min      2.740
_cell_volume                     2395(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11543
_diffrn_reflns_point_group_measured_fraction_full 0.804
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.770
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.41(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         6962
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1038P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.621
_reflns_Friedel_fraction_max     0.623
_reflns_number_gt                5153
_reflns_number_total             6962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce40855h.txt
_cod_data_source_block           MAC6'
_cod_original_formula_sum        'C20 H21 N6 O9.50 Zn2'
_cod_database_code               7210390
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.789
_shelxl_version_number           2013-2
_shelx_res_checksum              60690
_shelx_hkl_checksum              58448