Ligand effects on gas adsorption in nanoporous phthalocyanine crystals.
Stamos, Nikolaos-Angelos; McMonagle, Charles J.; Turner, Gemma F.; Allan, David R.; Warren, Mark R.; Warren, Anna J.; McKeown, Neil B.; Moggach, Stephen A.; Chemical communications (Cambridge, England) 60 (2024) 11508–11511; doi:10.1039/d4cc03896g

data_7133753
_publ_section_title
;
 Ligand effects on gas adsorption in nanoporous phthalocyanine crystals.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11508
_journal_page_last               11511
_journal_paper_doi               10.1039/d4cc03896g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Co2 C266.74 H288 N18 O16.74'
_chemical_formula_sum            'C266.74 H288 Co2 N18 O16.74'
_chemical_formula_weight         4131.84
_chemical_name_common            PNC[Co-cbipy-Co-vCO]
_chemical_name_systematic
;
bis(carbonyl(2,3,9,10,16,17,23,24-
octakis(2',6'-di-isopropylphenoxy)phthalocyaninato)-cobalt) 
4,4'-bipyridine unknown solvate
;
_space_group_crystal_system      cubic
_space_group_IT_number           222
_space_group_name_Hall           '-P 4a 2bc 3'
_space_group_name_H-M_alt        'P n -3 n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   37.9438(2)
_cell_length_b                   37.9438(2)
_cell_length_c                   37.9438(2)
_cell_measurement_reflns_used    4769
_cell_measurement_temperature    180
_cell_measurement_theta_max      20.136
_cell_measurement_theta_min      1.274
_cell_volume                     54628.9(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Diamond Light Source I19-2'
_diffrn_measurement_method       /w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            167605
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.136
_diffrn_reflns_theta_max         20.136
_diffrn_reflns_theta_min         1.274
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   AIMLESS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.754
_exptl_crystal_description       cube
_exptl_crystal_F_000             13214.16
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL shelxt in P n -3 n :2
CELL   37.9438   37.9438   37.9438     90.00     90.00     90.00
SPGR Pn-3n
C101 0.555 0.073 0.291 !       1.74 eA-3
C102 0.076 0.925 0.793 !       1.61 eA-3
C103 0.202 0.695 0.645 !       1.44 eA-3
C104 0.500 0.500 0.500 !       1.10 eA-3
Q105 0.305 0.816 0.326 !       1.10 eA-3
C106 1.000 1.000 1.000 !       1.10 eA-3
Q107 0.250 0.250 0.570 !       1.09 eA-3
Q108 0.149 0.803 0.233 !       0.94 eA-3
C109 0.750 0.750 0.789 !       0.85 eA-3
C110 0.997 0.343 0.180 !       0.80 eA-3
C111 1.003 0.657 0.820 !       0.80 eA-3
C112 0.179 0.347 0.500 !       0.80 eA-3
C113 0.162 0.168 0.507 !       0.79 eA-3
Q114 0.717 0.158 0.275 !       0.78 eA-3
C115 0.165 0.354 0.506 !       0.74 eA-3
C116 0.505 0.299 0.166 !       0.62 eA-3
Q117 0.619 0.500 0.241 !       0.60 eA-3
C118 0.809 0.232 0.845 !       0.58 eA-3
C119 0.487 0.625 0.790 !       0.57 eA-3
Q120 0.702 0.005 0.987 !       0.56 eA-3
C121 0.747 0.351 0.285 !       0.54 eA-3
Q122 0.073 0.406 0.553 !       0.54 eA-3
Q123 0.258 0.510 0.914 !       0.54 eA-3
C124 0.717 0.490 0.843 !       0.52 eA-3
C125 0.687 0.492 0.853 !       0.51 eA-3
Q126 0.202 0.768 0.173 !       0.51 eA-3
C127 0.243 0.362 0.994 !       0.50 eA-3
;
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00009(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4769
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1181P)^2^+136.6257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3653
_reflns_number_total             4769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03896g2.cif
_cod_data_source_block           3bipyCO
_cod_depositor_comments
'Adding full bibliography for 7133746--7133756.cif.'
_cod_original_cell_volume        54628.9(9)
_cod_original_sg_symbol_H-M      'P n -3 n'
_cod_original_formula_sum        'Co2 C266.74 H288 N18 O16.74'
_cod_database_code               7133753
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-O6
 1.12 with sigma of 0.02
 Co1-C15
 1.75 with sigma of 0.05
 C33-C35 \\sim C33-C35A
 with sigma of 0.02
 C30-C32 \\sim C30-C32A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C12) = Uanis(C17) = Uanis(C16) = Uanis(C15A) = Uanis(C14)
Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C24) = Uanis(C25) = Uanis(C26)
4. Rigid body (RIGU) restrains
 Co1, N2, N3, O2, C10, C4, C6, C5, C9, C7, C11, C8, C13, C12, C17, C16, C15A,
 C14, C18, C21, C19, C20, C22, C23, O1, N1, C1, C3, C2, C27, C28, C29, C24, C25,
  C26, C30, C31, C33, C34, C35, C32, C15, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 2*[Sof(H33)+Sof(C35)+Sof(H35A)+Sof(H35B)+Sof(H35C)+Sof(C35A)+Sof(H35D)+
 Sof(H35E)+Sof(H35F)]=1 with esd of 0.01
 2*[Sof(H30)+Sof(H30A)+Sof(C32)+Sof(H32A)+Sof(H32B)+Sof(H32C)+Sof(C32A)+
 Sof(H32D)+Sof(H32E)+Sof(H32F)]=1 with esd of 0.01
 Sof(H33)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Sof(H30A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(2)
 Sof(H30)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
 Fixed Sof: C3(0.5) H3(0.5) C2(0.5) H2(0.5) C15(0.09279) O6(0.09279)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C30(H30A), C33(H33)
6.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C32(H32A,
 H32B,H32C), C35A(H35D,H35E,H35F), C32A(H32D,H32E,H32F)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C16(H16), C15A(H15A), C14(H14), C3(H3), C2(H2), C27(H27),
 C28(H28), C26(H26)
6.d Fitted hexagon refined as free rotating group:
 C13(C12,C17,C16,C15A,C14), C27(C28,C29,C24,C25,C26)
;
_shelx_res_checksum              75960
_shelx_hkl_checksum              1708
_shelx_fab_checksum              80151
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'