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_1540551
_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, 10(C2 F6 N O4 S2), 2(C F3 O3 S)'
_chemical_formula_sum            'C202 H146 F40 N62 O66 S22 Zn9'
_chemical_formula_weight         6551.45
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   36.800(17)
_cell_length_b                   36.800(17)
_cell_length_c                   35.22(2)
_cell_measurement_reflns_used    6607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.728
_cell_measurement_theta_min      4.435
_cell_volume                     41306(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            122626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        16.000
_diffrn_reflns_theta_max         15.997
_diffrn_reflns_theta_min         0.619
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       needle
_exptl_crystal_F_000             19812
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.003
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         7400
_refine_ls_number_restraints     3287
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^-0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.2655
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5698
_reflns_number_total             7400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03926f2.cif
_cod_data_source_block           csw3108_sq_d
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-11
;
_cod_original_cell_volume        41306(45)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               1540551
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2014/6
_shelx_res_checksum              77730
_shelx_hkl_checksum              78880