Dual stimuli-induced formation of a μ-hydroxido bridged [Zn9L5(μ-OH)6]12+half-pipe
Wood, Christopher; Ronson, Tanya; McConnell, Anna; Roberts, Derrick A.; Nitschke, Jonathan; Chem. Sci.  (2015) –; doi:10.1039/C5SC03926F

data_1540552
_publ_section_title
;
 Dual stimuli-induced formation of a \m-hydroxido bridged
 [Zn9L5(\m-OH)6]12+half-pipe
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C5SC03926F
_journal_year                    2015
_chemical_formula_moiety
'C180 H146 N30 O16 Zn9, 8(C2 F6 N O4 S2), 4(O4 Re), C2 H3 N'
_chemical_formula_sum            'C198 H149 F48 N39 O64 Re4 S16 Zn9'
_chemical_formula_weight         6856.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.6360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.4811(16)
_cell_length_b                   22.2330(9)
_cell_length_c                   33.8318(14)
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      93.632
_cell_measurement_theta_min      4.929
_cell_volume                     26095.5(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            131433
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        47.440
_diffrn_reflns_theta_max         47.438
_diffrn_reflns_theta_min         2.360
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.636
_exptl_absorpt_correction_T_max  0.7493
_exptl_absorpt_correction_T_min  0.6123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             13520
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2260
_refine_ls_number_reflns         23676
_refine_ls_number_restraints     5215
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1616P)^2^+31.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16225
_reflns_number_total             23676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03926f2.cif
_cod_data_source_block           jn1501_sq_d
_cod_database_code               1540552
_shelx_estimated_absorpt_t_min   0.498
_shelx_estimated_absorpt_t_max   0.688
_shelxl_version_number           2014/6
_shelx_res_checksum              17194
_shelx_hkl_checksum              46011