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_1540549
_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, 12(Cl O4), 11(C2 H3 N), 6(H2 O) 
;
_chemical_formula_sum            'C202 H191 Cl12 N41 O70 Zn9'
_chemical_formula_weight         5326.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                81.86(3)
_cell_angle_beta                 81.60(3)
_cell_angle_gamma                75.35(3)
_cell_formula_units_Z            2
_cell_length_a                   19.431(4)
_cell_length_b                   22.435(5)
_cell_length_c                   28.802(6)
_cell_measurement_reflns_used    297833
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     11945(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f 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  0.1287
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            120107
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.390
_diffrn_reflns_theta_max         20.389
_diffrn_reflns_theta_min         1.733
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       plate
_exptl_crystal_F_000             5448
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2984
_refine_ls_number_reflns         23478
_refine_ls_number_restraints     2497
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1170P)^2^+52.0756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.2252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14941
_reflns_number_total             23478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03926f2.cif
_cod_data_source_block           jn1301
_cod_database_code               1540549
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2014/6
_shelx_res_checksum              97235
_shelx_hkl_checksum              52502