A Multistimulus Responsive Porous Coordination Polymer: Temperature-Mediated Control of Solid-State [2+2] Cycloaddition.
Claassens, Isabella E.; Barbour, Leonard J.; Haynes, Delia A.; Journal of the American Chemical Society 141 (2019) 11425–11429; doi:10.1021/jacs.9b05961

data_4127393
_publ_section_title
;
 A Multistimulus Responsive Porous Coordination Polymer:
 Temperature-Mediated Control of Solid-State [2+2] Cycloaddition.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11425
_journal_page_last               11429
_journal_paper_doi               10.1021/jacs.9b05961
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'Cd2 C68 H48 N4 O10, 4(C4 H9 N O)'
_chemical_formula_sum            'C76 H66 Cd2 N6 O12'
_chemical_formula_weight         1480.14
_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
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                114.710(2)
_cell_angle_beta                 107.275(2)
_cell_angle_gamma                95.625(2)
_cell_formula_units_Z            2
_cell_length_a                   20.0731(12)
_cell_length_b                   15.4449(9)
_cell_length_c                   15.1647(8)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.65
_cell_volume                     3942.3(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics
'X-Seed (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  EnCifer
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66025
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.105
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         2.180
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       'rhombohedral plate'
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         13961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+7.6674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9332
_reflns_number_total             13961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05961_si_002.cif
_cod_data_source_block           CdPCP_P2_irrad_100K_298K
_cod_database_code               4127393
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              18622
_shelx_hkl_checksum              91292
_shelx_fab_checksum              86387