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_7234694
_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         'C40 H32 O14, 4(C5 H7 N2), 4(O)'
_chemical_formula_sum            'C60 H68 N8 O18'
_chemical_formula_weight         1189.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.183(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7720(18)
_cell_length_b                   11.6573(12)
_cell_length_c                   29.512(3)
_cell_measurement_reflns_used    3125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.56
_cell_measurement_theta_min      2.34
_cell_volume                     5998.0(11)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1060
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40470
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        20.813
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_min         1.407
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3790
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce01326a1.cif
_cod_data_source_block           6
_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               7234694
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O16) = Uanis(O17)
Uanis(O18) = Uanis(O19)
Uanis(O20) = Uanis(O21)
3. Others
 Fixed Sof: O16(0.5) O17(0.5) O21(0.5) O20(0.5) O18(0.5) O19(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), N3(H3), C4(H4), N5(H5), N7(H7), C9(H9), C11(H11), C16(H16),
 C18(H18), C23(H23), C25(H25), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
  C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55),
 C57(H57), C58(H58), C59(H59), C60(H60)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6A,H6B), N8(H8A,H8B)
;
_olex2_submission_special_instructions 'No special instructions were received'