Host?guest assembly of ligand systems for metal ion complexation; synergistic solvent extraction of copper(ii) ions by N3O2-donor macrocycles and carboxylic or phosphinic acids
Byriel, Karl A.; Gasperov, Vesna; Gloe, Karsten; Kennard, Colin H. L.; Leong, Anthony J.; Lindoy, Leonard F.; Mahinay, Myrna S.; Pham, Huong T.; Tasker, Peter A.; Thorp, Derek; Turner, Peter; Dalton Transactions  (2003) 3034–; doi:10.1039/b303825d

data_7013054
_publ_section_title
;
 Host?guest assembly of ligand systems for metal ion complexation;
 synergistic solvent extraction of copper(ii) ions by N3O2-donor
 macrocycles and carboxylic or phosphinic acids
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              3034
_journal_paper_doi               10.1039/b303825d
_journal_year                    2003
_chemical_formula_sum            'C42 H56 N3 O9'
_chemical_formula_weight         746.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.528(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.638(10)
_cell_length_b                   12.575(7)
_cell_length_c                   19.075(10)
_cell_measurement_reflns_used    972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.373
_cell_measurement_theta_min      2.383
_cell_volume                     4099(4)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
teXsan for Windows (MSC, 1997), XSHELL (Bruker, 2000)
and WinGX (Farrugia, 1999)

;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35320
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0.03
_diffrn_standards_number         286
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian (XPREP, Bruker 1995; Coppens et al., 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.465
_exptl_crystal_size_min          0.237
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9213
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0400P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                6981
_reflns_number_total             9213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303825d.txt
_cod_data_source_block           lfl43
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_database_code               7013054