Mixed valence mono- and hetero-metallic grid catenanes
Giri, Chandan; Topić, Filip; Cametti, Massimo; Rissanen, Kari; Chem. Sci. 6 (2015) 5712–; doi:10.1039/C5SC01851J

data_1520709
_publ_section_title
;
 Mixed valence mono- and hetero-metallic grid catenanes
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5712
_journal_paper_doi               10.1039/C5SC01851J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
'2(C160 H106 Cu2 N48 O40 S8 Zn6), 11.5 Na, 1.65(C3 H7 N O), O33.9'
_chemical_formula_sum
'C324.95 H223.55 Cu4 N97.65 Na11.5 O115.55 S16 Zn12'
_chemical_formula_weight         9160.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-08 deposited with the CCDC.
2015-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2694(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.91216(13)
_cell_length_b                   32.64068(17)
_cell_length_c                   35.0386(2)
_cell_measurement_reflns_used    38303
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      74.2200
_cell_measurement_theta_min      3.3000
_cell_volume                     24800.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            79830
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.750
_diffrn_reflns_theta_max         67.749
_diffrn_reflns_theta_min         3.315
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9279.4
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.347(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5333
_refine_ls_number_reflns         52904
_refine_ls_number_restraints     6844
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1566P)^2^+2.8606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                48845
_reflns_number_total             52904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc01851j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1520709--1520712.cif.'
_cod_original_formula_sum
'C324.95 H223.55 Cu4 N97.65 Na11.50 O115.55 S16 Zn12'
_cod_database_code               1520709
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.834
_shelxl_version_number           2013-4
_shelx_res_checksum              92707
_shelx_hkl_checksum              88912
_shelx_fab_checksum              26932