A propanol-seamed C-methylcalix[4]resorcinarene hexamer accessible via solution crystallization, liquid-assisted grinding and vapour sorption
Payne, Richard M.; Oliver, Clive L.; CrystEngComm  (2018) –; doi:10.1039/C8CE00294K

data_7230210
_publ_section_title
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 A propanol-seamed C-methylcalix[4]resorcinarene hexamer accessible via
 solution crystallization, liquid-assisted grinding and vapour sorption
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00294K
_journal_year                    2018
_chemical_formula_moiety         'C32 H32 O8, 3(C3 H8 O), 1.67(O)'
_chemical_formula_sum            'C41 H59.33 O12.67'
_chemical_formula_weight         754.88
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-28 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.6175(18)
_cell_length_b                   33.6175(18)
_cell_length_c                   20.9185(13)
_cell_measurement_reflns_used    4117
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.40
_cell_volume                     20473(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.624
_diffrn_reflns_theta_min         1.199
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0745 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.8895. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             7320
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         13326
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.2085
_refine_ls_R_factor_gt           0.1158
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3286
_refine_ls_wR_factor_ref         0.3975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             13326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00294k2.cif
_cod_data_source_block           173k_sq
_cod_original_cell_volume        20473(3)
_cod_database_code               7230210
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.955
_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) groups
2. Restrained distances
 C1C-O1C
 1.41 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3C \\sim O1C \\sim C1C \\sim C2C \\sim C3A \\sim O1A \\sim C1A \\sim C2A \\sim
C2B1 \\sim O1B1 \\sim C1B1 \\sim C3B1 \\sim C3B2 \\sim O1B2 \\sim C1B2 \\sim
C2B2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C3C, O1C, C1C, C2C, C2A, O1A, C1A, C3A, C2B1, O1B1, C1B1, C3B1, C3B2, O1B2,
 C1B2, C2B2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1A, C1A, C2A, C3A} sigma for 1-2: 0.01, 1-3: 0.02
as
{O1B1, C1B1, C2B1, C3B1}
{O1A, C1A, C2A, C3A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1B2, C1B2, C2B2, C3B2}
{O1A, C1A, C2A, C3A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1C, C1C, C2C, C3C}
6. Others
 Sof(O1B2)=Sof(H1B2)=Sof(C1B2)=Sof(H1BC)=Sof(H1BD)=Sof(C2B2)=Sof(H2BC)=
 Sof(H2BD)=Sof(C3B2)=Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=1-FVAR(1)
 Sof(O1B1)=Sof(H1B1)=Sof(C1B1)=Sof(H1BA)=Sof(H1BB)=Sof(C2B1)=Sof(H2BA)=
 Sof(H2BB)=Sof(C3B1)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C7(H7A), C15(H15), C23(H23), C31(H31)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C1B1(H1BA,H1BB), C2B1(H2BA,H2BB), C1B2(H1BC,
 H1BD), C2B2(H2BC,H2BD), C1C(H1CA,H1CB), C2C(H2CA,H2CB)
7.c Me refined with riding coordinates:
 C3A(H3AA,H3AB,H3AC), C3B1(H3BA,H3BB,H3BC), C3B2(H3BD,H3BE,H3BF), C3C(H3CA,
 H3CB,H3CC)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C5(H5A), C10(H10), C13(H13), C18(H18), C21(H21), C26(H26), C29(H29)
7.e Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B1(H1B1), O1B2(H1B2), O1C(H1C)
7.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), O7(H7), O8(H8)
;
_shelx_res_checksum              48884
_shelx_fab_checksum              49065
_olex2_submission_special_instructions 'No special instructions were received'