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_7707118
_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
'C360 H392 Cl8 Co32 N16 O80 S32, 8(C5 H9 N O)'
_chemical_formula_sum            'C400 H464 Cl8 Co32 N24 O88 S32'
_chemical_formula_weight         10211.20
_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   mixed
_audit_creation_date             2020-12-03
_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                 143.163(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   66.638(2)
_cell_length_b                   51.3655(4)
_cell_length_c                   36.3667(12)
_cell_measurement_reflns_used    39366
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.4670
_cell_measurement_theta_min      2.2650
_cell_volume                     74630(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       84
_diffrn_reflns_limit_h_min       -82
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            214522
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.943
_diffrn_reflns_theta_min         2.187
_exptl_absorpt_coefficient_mu    6.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.909
_exptl_crystal_description       block
_exptl_crystal_F_000             20992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
A solvent mask was calculated and 8584 electrons were found in a volume of 39420\%A^3^ in 25 void per unit cell. This is consistent with the presence of 35[C5H9NO] or 50[C3H7NO] per Formula Unit which account for 8432 or 8528 electrons per unit cell, respectively.
;
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2778
_refine_ls_number_reflns         73304
_refine_ls_number_restraints     680
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38706
_reflns_number_total             73304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00556a2.cif
_cod_data_source_block           Co32-A
_cod_depositor_comments
'Adding full bibliography for 7707115--7707120.cif.'
_cod_original_cell_volume        74630(8)
_cod_database_code               7707118
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.547
_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, All O(H,H) groups
2. Restrained distances
 N11-C155 = N11-C148
 1.47 with sigma of 0.01
 C155-C130 = C136-C130 = C148-C136
 1.54 with sigma of 0.01
 O43-C148
 1.21 with sigma of 0.01
 N12-C203 = N12-C201
 1.47 with sigma of 0.01
 C204-C203 = C201-C202 = C204-C202
 1.54 with sigma of 0.01
 C175-C171
 2.5 with sigma of 0.01
 C199-C197 = C200-C197 = C198-C197
 1.54 with sigma of 0.01
 C199-C200 = C200-C198
 2.51 with sigma of 0.01
 C77-C124 = C174-C124 = C172-C124 = C167-C124
 1.54 with sigma of 0.01
 C172-C174 = C174-C167
 2.51 with sigma of 0.01
 C207-C209 = C209-C208
 2.51 with sigma of 0.01
 C121-C206 = C209-C206 = C207-C206 = C208-C206
 1.54 with sigma of 0.01
 C211-C212 = C212-C210
 2.51 with sigma of 0.01
 C143-N10 = N10-C145
 1.47 with sigma of 0.01
 C105-C168 \\sim C105-C187
 with sigma of 0.02
 C105-C170 \\sim C105-C185
 with sigma of 0.02
 C105-C184 \\sim C105-C186
 with sigma of 0.02
 C140-C191 \\sim C140-C196
 with sigma of 0.02
 C140-C192 \\sim C140-C194
 with sigma of 0.02
 C140-C193 \\sim C140-C195
 with sigma of 0.02
 C126-C179 \\sim C126-C189
 with sigma of 0.02
 C126-C181 \\sim C126-C190
 with sigma of 0.02
 C126-C182 \\sim C126-C188
 with sigma of 0.02
 C206-C207 \\sim C206-C210
 with sigma of 0.02
 C206-C208 \\sim C206-C211
 with sigma of 0.02
 C206-C209 \\sim C206-C212
 with sigma of 0.02
3. Rigid bond restraints
 O43, C148
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C90, C198, C197, C200, C199
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C177 \\sim C122 \\sim C166 \\sim C146: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C105 \\sim C168 \\sim C170 \\sim C184 \\sim C185 \\sim C186 \\sim C187: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C88 \\sim C106 \\sim C153 \\sim C158 \\sim C160: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C127 \\sim C68 \\sim C147 \\sim C161 \\sim C165: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C138 \\sim C118 \\sim C163 \\sim C176 \\sim C178: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
O43 \\sim C148 \\sim C155 \\sim N11 \\sim C130 \\sim C136 \\sim C173: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
C140 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim C196: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C204 \\sim C202 \\sim C201 \\sim C203 \\sim N12 \\sim C205 \\sim O44: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C84 \\sim C131 \\sim C150 \\sim C171 \\sim C175: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C181 \\sim C182 \\sim C179 \\sim C126: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C190 \\sim C188 \\sim C126 \\sim C189: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C197 \\sim C198 \\sim C199 \\sim C200: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C124 \\sim C167 \\sim C174: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C174 \\sim C124 \\sim C167 \\sim C172: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C169 \\sim C151 \\sim C180 \\sim C119 \\sim C183: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C206 \\sim C207 \\sim C208 \\sim C209 \\sim C210 \\sim C211 \\sim C212: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C107 \\sim C42 \\sim C152 \\sim C156 \\sim C162: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C179, C181, C182
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C192, C193, C191
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C194, C196, C195
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C204, C202, C201, C203, N12, C205, O44
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C189, C190, C188
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C198, C197, C200, C199
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C174, C167, C172
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C207, C206, C209, C208
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C210, C206, C212, C211
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C185)=Sof(H18P)=Sof(H18Q)=Sof(H18R)=Sof(C186)=Sof(H18S)=Sof(H18T)=
 Sof(H18U)=Sof(C187)=Sof(H18V)=Sof(H18W)=Sof(H18X)=1-FVAR(1)
 Sof(C168)=Sof(H16V)=Sof(H16W)=Sof(H16X)=Sof(C170)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C184)=Sof(H18M)=Sof(H18N)=Sof(H18O)=FVAR(1)
 Sof(C188)=Sof(H18Y)=Sof(HI)=Sof(HJ)=Sof(C189)=Sof(H18Z)=Sof(HK)=Sof(HL)=
 Sof(C190)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(2)
 Sof(C179)=Sof(H17Y)=Sof(HG)=Sof(HH)=Sof(C181)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C182)=Sof(H18G)=Sof(H18H)=Sof(H18I)=FVAR(2)
 Sof(C194)=Sof(H19M)=Sof(H19N)=Sof(H19O)=Sof(C195)=Sof(H19P)=Sof(H19Q)=
 Sof(H19R)=Sof(C196)=Sof(H19S)=Sof(H19T)=Sof(H19U)=1-FVAR(3)
 Sof(C191)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C192)=Sof(H19G)=Sof(H19H)=
 Sof(H19I)=Sof(C193)=Sof(H19J)=Sof(H19K)=Sof(H19L)=FVAR(3)
 Sof(C210)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C211)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=Sof(C212)=Sof(H21G)=Sof(H21H)=Sof(H21I)=1-FVAR(4)
 Sof(C207)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C208)=Sof(H20G)=Sof(H20H)=
 Sof(H20I)=Sof(C209)=Sof(H20J)=Sof(H20K)=Sof(H20L)=FVAR(4)
7.a Riding coordinates:
 O33(H33A,H33B), O34(H34A,H34B), O35(H35A,H35B), O36(H36A,H36B), O37(H37A,
 H37B), O38(H38A,H38B), O39(H39A,H39B), O40(H40A,H40B), C132(H13A,H13B,H13C),
 C154(H15J,H15K,H15L), C159(H15S,H15T,H15U), C162(H16G,H16H,H16I), C167(H16S,
 H16T,H16U), C169(H16Y,HC,HD), C172(H17G,H17H,H17I), C174(H17J,H17K,H17L),
 C180(H18A,H18B,H18C), C183(H18J,H18K,H18L), C188(H18Y,HI,HJ), C189(H18Z,HK,HL),
  C190(H19A,H19B,H19C), C191(H19D,H19E,H19F), C192(H19G,H19H,H19I), C193(H19J,
 H19K,H19L), C194(H19M,H19N,H19O), C195(H19P,H19Q,H19R), C196(H19S,H19T,H19U),
 C198(H19V,H19W,H19X), C201(H20M,H20N), C202(H20O,H20P), C204(H20Q,H20R),
 C205(H20S,H20T,H20U), C207(H20D,H20E,H20F), C208(H20G,H20H,H20I), C209(H20J,
 H20K,H20L), C210(H21A,H21B,H21C), C211(H21D,H21E,H21F), C212(H21G,H21H,H21I)
7.b Secondary CH2 refined with riding coordinates:
 C130(H13M,H13N), C135(H13Q,H13R), C136(H13O,H13P), C141(H14G,H14H), C142(H14M,
 H14N), C144(H14I,H14J), C145(H14O,H14P), C149(H14K,H14L), C155(H15V,H15W)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C16(H16), C19(H19), C29(H29), C33(H33), C39(H39), C41(H41),
 C48(H48), C51(H51), C52(H52), C57(H57), C58(H58), C66(H66), C70(H70), C71(H71),
  C72(H72), C73(H73), C76(H76), C80(H80), C81(H81), C83(H83), C87(H87),
 C89(H89), C92(H92), C93(H93), C95(H95), C102(H102), C103(H103), C108(H108),
 C109(H109), C111(H111), C113(H113), C114(H114), C117(H117), C119(H119)
7.d Idealised Me refined as rotating group:
 C125(H12A,H12B,H12C), C128(H12D,H12E,H12F), C129(H12G,H12H,H12I), C133(H13D,
 H13E,H13F), C134(H13G,H13H,H13I), C137(H13J,H13K,H13L), C146(H14A,H14B,H14C),
 C147(H14D,H14E,H14F), C150(H15A,H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,
 H15H,H15I), C156(H15M,H15N,H15O), C157(H15X,H15Y,H), C158(H15P,H15Q,H15R),
 C160(H16A,H16B,H16C), C161(H16D,H16E,H16F), C163(H16J,H16K,H16L), C164(H16Z,HA,
 HB), C165(H16M,H16N,H16O), C166(H16P,H16Q,H16R), C168(H16V,H16W,H16X),
 C170(H17A,H17B,H17C), C171(H17D,H17E,H17F), C173(H17Z,HE,HF), C175(H17M,H17N,
 H17O), C176(H17P,H17Q,H17R), C177(H17S,H17T,H17U), C178(H17V,H17W,H17X),
 C179(H17Y,HG,HH), C181(H18D,H18E,H18F), C182(H18G,H18H,H18I), C184(H18M,H18N,
 H18O), C185(H18P,H18Q,H18R), C186(H18S,H18T,H18U), C187(H18V,H18W,H18X),
 C199(H19Y,HM,HN), C200(H20A,H20B,H20C)
;
_shelx_res_checksum              52144
_shelx_hkl_checksum              69627
_shelx_fab_checksum              7768
_platon_squeeze_void_probe_radius 1.20