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_7234693
_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         'C50 H42 Cu N2 O14, C6.33'
_chemical_formula_sum            'C55 H49 Cu N3 O14'
_chemical_formula_weight         1039.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8977(4)
_cell_length_b                   29.2369(9)
_cell_length_c                   12.7603(5)
_cell_measurement_temperature    100(2)
_cell_volume                     5557.9(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31696
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.883
_diffrn_reflns_theta_max         25.883
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0661 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.8848.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1304P)^2^+8.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3763
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01326a1.cif
_cod_data_source_block           7
_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               7234693
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(3)
 0.42(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C3-C19
 1.54 with sigma of 0.02
 C3-C20
 1.54 with sigma of 0.02
 O4-C19
 1.25 with sigma of 0.02
 O5-C19
 1.25 with sigma of 0.02
 O7-C20
 1.25 with sigma of 0.02
 O6-C20
 1.25 with sigma of 0.02
4. Restrained planarity
 C3, C20, O6, O7
 with sigma of 0.01
 C30, C31, C32, C33, C34, C35
 with sigma of 0.01
5. 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(C3) = Uanis(C19) = Uanis(C20) = Uanis(O4) = Uanis(O5) = Uanis(O6) =
Uanis(O7)
Uiso(C34) = Uiso(C30) = Uiso(C31) = Uiso(C35) = Uiso(C32) = Uiso(C36) =
Uiso(C33) = Uiso(C37)
6. Others
 Fixed Sof: O4(0.5) O5(0.5) O6(0.5) O7(0.5) C19(0.5) C20(0.5) C31(0.5)
 C32(0.3333) C33(0.3333) C36(0.3333) C37(0.3333) C35(0.5) C34(0.3333)
7.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)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'