Highly branched and loop-rich gels via formation of metal-organic cages linked by polymers
Aleksandr V. Zhukhovitskiy; Mingjiang Zhong; Eric G. Keeler; Vladimir K. Michaelis; Jessie E. P. Sun; Michael J. A. Hore; Darrin J. Pochan; Robert G. Griffin; Adam P. Willard; Jeremiah A. Johnson; Nature Chemistry 8 (2016) 33–41; doi:10.1038/nchem.2390

data_1552053
_publ_section_title
;
 Highly branched and loop-rich gels via formation of metal-organic cages
 linked by polymers
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              33
_journal_page_last               41
_journal_paper_doi               10.1038/nchem.2390
_journal_volume                  8
_journal_year                    2016
_chemical_formula_sum            'C72.5 H40 N12.8 O22.91 Pd2'
_chemical_formula_weight         1669.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.134(2)
_cell_length_b                   15.1380(12)
_cell_length_c                   19.4067(14)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.76
_cell_volume                     8265.2(11)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1036
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            219815
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.275
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.788
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10556
_refine_ls_number_restraints     1060
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          6.596
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1534P)^2^+32.0449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2592
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7723
_reflns_number_total             10556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2390-s2.cif
_cod_data_source_block           X14074
_cod_original_cell_volume        8265.3(11)
_cod_original_formula_sum        'C72.50 H40 N12.80 O22.91 Pd2'
_cod_database_code               1552053
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2014/6
_shelx_res_checksum              24825
_shelx_hkl_checksum              50927