Design and Synthesis of Capped-Paddlewheel-Based Porous Coordination Cages
Lorzing, Gregory; Gosselin, Eric; Lindner, Brian S.; Bhattacharjee, Rameswar; Yap, Glenn; Caratzoulas, Stavros; Bloch, Eric D.; Chemical Communications  (2019) –; doi:10.1039/C9CC05002G

data_7123865
_publ_section_title
;
 Design and Synthesis of Capped-Paddlewheel-Based Porous Coordination
 Cages
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05002G
_journal_year                    2019
_chemical_formula_moiety         'C38 H42 Mo2 N8, 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H43.5 Mo2 N8.5'
_chemical_formula_weight         823.20
_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   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-04-26 deposited with the CCDC.    2019-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                64.0710(10)
_cell_angle_beta                 82.3250(10)
_cell_angle_gamma                89.9970(10)
_cell_formula_units_Z            4
_cell_length_a                   16.0829(5)
_cell_length_b                   18.2035(6)
_cell_length_c                   19.6805(7)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.59
_cell_measurement_theta_min      2.28
_cell_volume                     5124.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96943
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.125
_diffrn_reflns_theta_min         1.276
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         22619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13717
_reflns_number_total             22619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05002g2.cif
_cod_data_source_block           eric165_sq
_cod_original_formula_sum        'C39 H43.50 Mo2 N8.50'
_cod_database_code               7123865
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              55491
_shelx_fab_checksum              96943