Knock-on synthesis of tritopic calix[4]pyrrole host for enhanced anion interactions.
Chahal, Mandeep K.; Labuta, Jan; Březina, Václav; Karr, Paul A.; Matsushita, Yoshitaka; Webre, Whitney A.; Payne, Daniel T.; Ariga, Katsuhiko; D'Souza, Francis; Hill, Jonathan P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15583–15596; doi:10.1039/c9dt02365h

data_7700628
_publ_section_title
;
 Knock-on synthesis of tritopic calix[4]pyrrole host for enhanced anion
 interactions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15583
_journal_page_last               15596
_journal_paper_doi               10.1039/c9dt02365h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C83.2 H90.2 Cl0.6 N10 Ni O4'
_chemical_formula_weight         1374.23
_chemical_name_common            Spiro_fused_OxPNi
_chemical_properties_physical    Photo-sensitive
_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   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-07-11 deposited with the CCDC.    2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1354(5)
_cell_length_b                   14.6714(4)
_cell_length_c                   32.6068(9)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      2.27
_cell_volume                     8604.9(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_molecular_graphics
;
'shelXle ver. 958, Huebschle et al., 2011)'
;
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67128
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.352
_diffrn_reflns_theta_max         20.352
_diffrn_reflns_theta_min         1.791
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.5946
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       Bar
_exptl_crystal_F_000             2918
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         8426
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+18.9925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6793
_reflns_number_total             8426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02365h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7700628.cif.'
_cod_original_formula_sum        'C83.20 H90.20 Cl0.60 N10 Ni O4'
_cod_database_code               7700628
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              65613
_shelx_fab_checksum              65225