Structure and Dynamics of Metallomacrocycles: Recognition of Zinc Xylyl-Bicyclam by an HIV Coreceptor
Xiangyang Liang; John A. Parkinson; Michael Weishäupl; Robert O. Gould; Stephen J. Paisey; Hye-seo Park; Tina M. Hunter; Claudia A. Blindauer; Simon Parsons; Peter J. Sadler; Journal of the American Chemical Society 124 (2002) 9105–9112; doi:10.1021/ja0260723

data_4115005
_publ_section_title
;
 Structure and Dynamics of Metallomacrocycles: Recognition of Zinc
 Xylyl-Bicyclam by an HIV Coreceptor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9105
_journal_page_last               9112
_journal_paper_doi               10.1021/ja0260723
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '[Pd(cyclam)](OAc)2.2H2O'
_chemical_formula_sum            'C14 H34 N4 O6 Pd'
_chemical_formula_weight         460.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.521(2)
_cell_angle_beta                 86.559(2)
_cell_angle_gamma                89.682(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5829(10)
_cell_length_b                   9.7811(12)
_cell_length_c                   11.6962(14)
_cell_measurement_reflns_used    3349
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      53
_cell_measurement_theta_min      5
_cell_volume                     973.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7978
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       Plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       SHELXTL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment
;
riding,rotating groups me, freely refined H on N and O
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                3088
_reflns_number_total             3947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0260723_s4.cif
_cod_data_source_block           recoth
_cod_database_code               4115005