Synthesis, Cu(ii) complexation, (64)Cu-labeling and biological evaluation of cross-bridged cyclam chelators with phosphonate pendant arms.
Ferdani, Riccardo; Stigers, Dannon J.; Fiamengo, Ashley L.; Wei, Lihui; Li, Barbara T. Y.; Golen, James A.; Rheingold, Arnold L.; Weisman, Gary R.; Wong, Edward H.; Anderson, Carolyn J.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1938–1950; doi:10.1039/c1dt11743b

data_7017955
_publ_section_title
;
 Synthesis, Cu(ii) complexation, (64)Cu-labeling and biological evaluation
 of cross-bridged cyclam chelators with phosphonate pendant arms.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1938
_journal_page_last               1950
_journal_paper_doi               10.1039/c1dt11743b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C15 H40 Cu N4 O10.5 P'
_chemical_formula_weight         539.02
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            8
_cell_length_a                   10.1989(19)
_cell_length_b                   35.067(7)
_cell_length_c                   12.943(3)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.61
_cell_volume                     4629.0(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            57822
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.9003
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+17.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                4831
_reflns_number_total             5510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11743b.txt
_cod_data_source_block           wong190
_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_values 1715 2011-07-08 13:25:40Z adriana 

2018-03-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4629.2(15)
_cod_original_sg_symbol_H-M      Pccn
_cod_original_formula_sum        'C30 H80 Cu2 N8 O21 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1078.04
_cod_database_code               7017955