Oxovanadium(IV) Cyclam and Bicyclam Complexes: Potential CXCR4 Receptor Antagonists
Allison Ross; Dinesh C. Soares; Danielle Covelli; Christophe Pannecouque; Laura Budd; Anna Collins; Neil Robertson; Simon Parsons; Erik De Clercq; Pierre Kennepohl; Peter J. Sadler; Inorganic Chemistry 49 (2010) 1122–1132; doi:10.1021/ic9020614

data_4314688
_publ_contact_author_address
; 
 Department of Chemistry, 
 Joseph Black Builing, 
 West Mains Road, 
 University of Edinburgh, 
 Edinburgh, EH9 3JJ, UK. 
;
_publ_contact_author_email       anna.collins@ed.ac.uk
_publ_contact_author_name        'Anna Collins'
_publ_contact_author_phone       '+44 131 650 4806'
_publ_section_title
;
 Oxovanadium(IV) Cyclam and Bicyclam Complexes: Potential CXCR4 Receptor
 Antagonists
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1122
_journal_page_last               1132
_journal_paper_doi               10.1021/ic9020614
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'Allison Ross, ARVC(Cl)1'
_chemical_formula_moiety
'C10 H24 Cl N4 O1 V1, Cl, (C H4 O), 1.5(H2 O)'
_chemical_formula_sum            'C34 H84 N12 O19 S3 V3'
_chemical_formula_weight         1214.13
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-06-06
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.2262(2)
_cell_length_b                   25.2262(2)
_cell_length_c                   15.1963(3)
_cell_measurement_reflns_used    6234
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     8374.76(19)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55545
_diffrn_reflns_theta_full        30.495
_diffrn_reflns_theta_max         30.495
_diffrn_reflns_theta_min         2.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             3846.000
_exptl_crystal_recrystallization_method
; 
Diffusion of ether into methanol at 277K.
 
;
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.010(18)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9316
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.000409
_refine_ls_structure_factor_coef Fsqd
_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: 
 49.5 80.6 50.6 23.0 5.30 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0849
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0849
_reflns_limit_h_max              0
_reflns_limit_h_min              -31
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -21
_reflns_number_gt                3992
_reflns_number_total             5575
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.13684(5)
_cod_data_source_file            ic9020614_si_002_2.cif
_cod_data_source_block           ps6027
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R 3 c '
_cod_database_code               4314688