Cascade chemistry in azacryptand cages: bridging carbonates and methylcarbonates
Yann Dussart; Charlie Harding; Pia Dalgaard; Christine McKenzie; Renuka Kadirvelraj; Vickie McKee; Jane Nelson; J. Chem. Soc., Dalton Trans.  (2002) 1704–1713; doi:10.1039/b110449g

data_7011323
_publ_section_title
;
 Cascade chemistry in azacryptand cages: bridging carbonates and
 methylcarbonates
;
_journal_issue                   8
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1704
_journal_page_last               1713
_journal_paper_doi               10.1039/b110449g
_journal_year                    2002
_chemical_formula_sum            'C39.5 H65 Cl2 N8 Ni2 O14'
_chemical_formula_weight         1064.32
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.320(3)
_cell_length_b                   10.8310(16)
_cell_length_c                   19.546(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.22
_cell_volume                     5148.6(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       -1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4533
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.06
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.8524
_exptl_absorpt_correction_T_min  0.7654
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.96(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+2.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                3112
_reflns_number_total             4308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110449g.txt
_cod_data_source_block           Complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5148.5(11)
_cod_original_sg_symbol_H-M      Pca21
_cod_original_formula_sum        'C39.50 H65 Cl2 N8 Ni2 O14'
_cod_database_code               7011323