A novel series of giant cobalt-calixarene macrocycles: ring-expansion and modulation of pore apertures through recrystallization.
Zhang, Kai; Du, Shao-Wu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6181–6187; doi:10.1039/d1dt00556a

data_7707117
_publ_section_title
;
 A novel series of giant cobalt-calixarene macrocycles: ring-expansion and
 modulation of pore apertures through recrystallization.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6181
_journal_page_last               6187
_journal_paper_doi               10.1039/d1dt00556a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C306 H318 Co30 N24 O90 S24, 6[C2H8N]'
_chemical_formula_sum            'C318 H366 Co30 N30 O90 S24'
_chemical_formula_weight         8586.00
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.3887(2)
_cell_length_b                   37.3887(2)
_cell_length_c                   37.3887(2)
_cell_measurement_reflns_used    19150
_cell_measurement_temperature    110.3(2)
_cell_measurement_theta_max      48.3720
_cell_measurement_theta_min      2.1020
_cell_volume                     52266.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.3(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  23.00   0.50    1.72    --   -1.72 -85.00 170.00   80
  2  \w    107.00 137.00   0.50    6.50    --   72.03 121.00 178.00   60
  3  \w    -50.00  -9.00   0.50    6.50    --  -75.46  44.00-121.00   82
  4  \w    -26.00   0.00   0.50    6.50    --  -75.46  19.00 -30.00   52
  5  \w    -26.00  -1.00   0.50    6.50    --  -75.46  19.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203295000
_diffrn_orient_matrix_UB_12      -0.0260803000
_diffrn_orient_matrix_UB_13      0.0138179000
_diffrn_orient_matrix_UB_21      -0.0244593000
_diffrn_orient_matrix_UB_22      0.0242847000
_diffrn_orient_matrix_UB_23      0.0098945000
_diffrn_orient_matrix_UB_31      -0.0165311000
_diffrn_orient_matrix_UB_32      -0.0038108000
_diffrn_orient_matrix_UB_33      -0.0314763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            82632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.840
_diffrn_reflns_theta_min         2.055
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    5.960
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             16944
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
A solvent mask was calculated and 5853 electrons were found in a volume of  19870\%A^3^ in 5 void per unit cell. This is consistent with the presence of 6[C2H8N], 27[C3H7NO], or 6[C2H8N], 50[CH4O] per Formula Unit which account for 5832 or 5848 electrons per unit cell, respectively.
;
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.505
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         19762
_refine_ls_number_restraints     1861
_refine_ls_restrained_S_all      1.521
_refine_ls_R_factor_all          0.2575
_refine_ls_R_factor_gt           0.1571
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4410
_refine_ls_wR_factor_ref         0.4962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7810
_reflns_number_total             19762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00556a2.cif
_cod_data_source_block           Co30-B
_cod_depositor_comments
'Adding full bibliography for 7707115--7707120.cif.'
_cod_original_cell_volume        52266.2(8)
_cod_database_code               7707117
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C30-C29 = C38-C30 = C37-C30
 1.54 with sigma of 0.01
 C44-C26
 1.47 with sigma of 0.01
 C51-C48 = C50-C48 = C49-C48
 1.54 with sigma of 0.01
 C43-C41 = C40-C41 = C41-C42
 1.54 with sigma of 0.01
 C44-C47 = C44-C46 = C44-C45
 1.54 with sigma of 0.01
 C29-C37 \\sim C37-C38 \\sim C38-C29
 with sigma of 0.02
 C51-C49 \\sim C49-C50 \\sim C50-C51
 with sigma of 0.02
 C40-C42 \\sim C42-C43 \\sim C43-C40
 with sigma of 0.02
 C46-C47 \\sim C47-C45 \\sim C45-C46
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim O1 \\sim O2 \\sim
O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11
\\sim O12 \\sim O13 \\sim O14 \\sim O15: within -3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C40(H40A,H40B,H40C), C45(H45A,H45B,H45C)
4.b Rotating group:
 O8(H8A,H8B), O13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C12(H12), C17(H17), C19(H19), C22(H22), C25(H25), C27(H27),
 C33(H33), C35(H35)
4.d Fitted pentagon refined as free rotating group:
 N3(N4,C1,C2,C3)
4.e Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C15(C16,C17,C18,C19,C20), C23(C24,C25,C26,C27,C28),
 C31(C32,C33,C34,C35,C36)
4.f Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              86456
_shelx_hkl_checksum              85068
_shelx_fab_checksum              32300
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.831