Controlling phase in low-nuclearity calixarene-capped porous coordination cages with ligand functionalization
Dworzak, Michael R.; Rowland, Casey A.; Yap, Glenn P. A.; Bloch, Eric D.; CrystEngComm  (2022) –; doi:10.1039/D2CE00861K

data_7245449
_publ_section_title
;
 Controlling phase in low-nuclearity calixarene-capped porous coordination
 cages with ligand functionalization
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00861K
_journal_year                    2022
_chemical_formula_moiety         'C142 H157 N6 Ni6 O38 S8, 16[C3H7NO]'
_chemical_formula_sum            'C190 H269 N22 Ni6 O54 S8'
_chemical_formula_weight         4334.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.204(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.824(10)
_cell_length_b                   23.576(5)
_cell_length_c                   40.269(9)
_cell_measurement_reflns_used    8728
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      58.89
_cell_measurement_theta_min      2.48
_cell_volume                     43449(16)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            95491
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        59.120
_diffrn_reflns_theta_max         59.120
_diffrn_reflns_theta_min         2.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1819 before and 0.1052 after correction.
The Ratio of minimum to maximum transmission is 0.6742.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             18328
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.691
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1819
_refine_ls_number_reflns         30269
_refine_ls_number_restraints     3177
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1925P)^2^+75.2762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3000
_refine_ls_wR_factor_ref         0.3344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16834
_reflns_number_total             30269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00861k2.cif
_cod_data_source_block           eric497
_cod_original_cell_volume        43450(16)
_cod_database_code               7245449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.632
_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
 C102-C104 = C102-C105 = C102-C103 = C67-C70
 1.534 with sigma of 0.02
 C104-C105 = C104-C103 = C105-C103
 -2.5 with sigma of 0.02
 C77-C78 \\sim C77-C79 \\sim C77-C80
 with sigma of 0.02
 C78-C79 \\sim C79-C80 \\sim C80-C78
 with sigma of 0.02
 C140-O18 \\sim C140-O38 \\sim C140-O28 \\sim C140-O19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O30 \\sim C140 \\sim N6 \\sim C141 \\sim C142: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O30, C140, N6, C141, C142
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Free rotating group:
 O30(C140,N6,C141,C142)
5.b Secondary CH2 refined with riding coordinates:
 C120(H12A,H12B)
5.c Me refined with riding coordinates:
 C141(H14A,H14B,H14C), C142(H14D,H14E,H14F), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C80(H80A,H80B,H80C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C105(H10J,
 H10K,H10L)
5.d Aromatic/amide H refined with riding coordinates:
 C140(H140), C2(H2), C4(H4), C12(H12), C14(H14), C22(H22), C24(H24), C32(H32),
 C34(H34), C42(H42), C44(H44), C52(H52), C54(H54), C62(H62), C64(H64), C72(H72),
  C74(H74), C83(H83), C85(H85), C86(H86), C89(H89), C90(H90), C92(H92),
 C95(H95), C96(H96), C97(H97), C99(H99), C100(H100), C108(H108), C110(H110),
 C111(H111), C114(H114), C115(H115), C117(H117), C121(H121), C122(H122),
 C124(H124), C125(H125), C131(H131), C134(H134), C137(H137)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C128(H12C,H12D,
 H12E), C129(H12F,H12G,H12H), C130(H13A,H13B,H13C), C132(H13D,H13E,H13F),
 C133(H13G,H13H,H13I), C135(H13J,H13K,H13L), C136(H13M,H13N,H13O), C138(H13P,
 H13Q,H13R), C139(H13S,H13T,H13U)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 5317 electrons were 
found in a volume of 19502\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
16[C3H7NO] per Asymmetric Unit 
which account for 5120 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61022
_shelx_hkl_checksum              1448
_shelx_fab_checksum              18506
_olex2_submission_special_instructions 'No special instructions were received'