Investigations into the assembly behaviour of a ‘rigidified’ p-carboxylatocalix[4]arene
Fairbairn, Robyn E.; Teat, Simon J.; Ling, Irene; Dalgarno, Scott J.; CrystEngComm 21 (2019) 6659–; doi:10.1039/C9CE01326A

data_7234692
_publ_section_title
;
 Investigations into the assembly behaviour of a
 &#x2018;rigidified&#x2019; p-carboxylatocalix[4]arene
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6659
_journal_paper_doi               10.1039/C9CE01326A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'0.5(C104 H100 Mn2 N4 O32), 0.5(C10 H10 N2), 4(O)'
_chemical_formula_sum            'C57 H65 Mn N3 O20'
_chemical_formula_weight         1167.06
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-08 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.647(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4398(5)
_cell_length_b                   27.9839(11)
_cell_length_c                   15.9403(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5546.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35944
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.030
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.9417.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.810
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0852
_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^)+(0.1702P)^2^+15.3898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2477
_refine_ls_wR_factor_ref         0.2733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4310
_reflns_number_total             5701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01326a1.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7234691--7234694.cif.
;
_cod_database_code               7234692
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C24
 1.39 with sigma of 0.02
 C24-C23
 1.39 with sigma of 0.02
 C23-C22
 1.39 with sigma of 0.02
 C21-C22
 1.39 with sigma of 0.02
 C25-N1
 1.39 with sigma of 0.02
 C21-N1
 1.39 with sigma of 0.02
 N36-C37
 1.39 with sigma of 0.02
 C37-C38
 1.39 with sigma of 0.02
 C40-C39
 1.39 with sigma of 0.02
 C38-C39
 1.39 with sigma of 0.02
 N36-C35
 1.39 with sigma of 0.02
 C40-C35
 1.39 with sigma of 0.02
 O8-C26
 1.45 with sigma of 0.02
 O8-C26A
 1.45 with sigma of 0.02
3. Restrained planarity
 C35, N36, C37, C38, C39, C40
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C35) = Uanis(N36) = Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40)
Uanis(O9) = Uanis(O9A) = Uanis(O10) = Uanis(O8) = Uanis(C26) = Uanis(C26A)
5. Others
 Fixed Sof: C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C40(0.5) H40(0.5) C38(0.5)
 H38(0.5) C39(0.5) H39(0.5) C37(0.5) H37(0.5) C35(0.5) H35(0.5) O9(0.5)
 O9A(0.5) C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B)
6.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C21(H21), C23(H23), C24(H24), C25(H25),
 C40(H40), C38(H38), C39(H39), C37(H37), C35(H35), C22(H22)
6.d Tetrahedral OH refined with riding coordinates:
 O5(H5)
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_olex2_submission_special_instructions 'No special instructions were received'