A dual-functional tetrakis-imidazolium macrocycle for supramolecular assembly
Serpell, Christopher J.; Cookson, James; Thompson, Amber L.; Beer, Paul D.; Chemical Science 2 (2011) 494–; doi:10.1039/c0sc00511h

data_1515510
_publ_section_title
;
 A dual-functional tetrakis-imidazolium macrocycle for supramolecular
 assembly
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              494
_journal_paper_doi               10.1039/c0sc00511h
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         '0.39(C41 H28 Co4 O18), C40 H36 N8, 4(F6 P)'
_chemical_formula_sum            'C56.15 H47.03 Co1.58 F24 N8 O7.09 P4'
_chemical_formula_weight         1620.12
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-04-18
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9688(10)
_cell_length_b                   18.0778(6)
_cell_length_c                   21.4031(7)
_cell_measurement_reflns_used    4682
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     8887.1(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8504
_diffrn_reflns_theta_full        25.354
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         5.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3260.474
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
After full modelling of the structure, some residual electron
density was observed, but could not be fitted to any sensible
solvent scheme. Instead, Platon Squeeze was used to include
this data in the refinement.
;
_refine_diff_density_max         1.93
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     427
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.1542
_refine_ls_shift/su_max          0.001629
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
3.78 2.46 2.05
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2606
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1803
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                4100
_reflns_number_total             4570
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.03
_oxford_diffrn_Wilson_scale      79.34
_oxford_refine_ls_r_factor_ref   0.1542
_oxford_refine_ls_scale          0.412(3)
_oxford_reflns_number_all        5596
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 012CJS08
_cod_data_source_file            c0sc00511h.txt
_cod_data_source_block           11
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'I b a m '
_cod_database_code               1515510