CXCR4 chemokine receptor antagonists: nickel(II) complexes of configurationally restricted macrocycles.
Smith, Rachel; Huskens, Dana; Daelemans, Dirk; Mewis, Ryan E.; Garcia, Courtney D.; Cain, Amy N.; Freeman, TaRynn N Carder; Pannecouque, Christophe; De Clercq, Erik; Schols, Dominique; Hubin, Timothy J.; Archibald, Stephen J.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11369–11377; doi:10.1039/c2dt31137b

data_7020263
_publ_section_title
;
 CXCR4 chemokine receptor antagonists: nickel(II) complexes of
 configurationally restricted macrocycles.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11369
_journal_page_last               11377
_journal_paper_doi               10.1039/c2dt31137b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C16 H35 F6 N4 Ni O3 P'
_chemical_formula_weight         535.16
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.005(2)
_cell_length_b                   26.005(2)
_cell_length_c                   17.2968(11)
_cell_measurement_reflns_used    6355
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.76
_cell_measurement_theta_min      2.52
_cell_volume                     10130.0(13)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP III (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-II image plate'
_diffrn_measurement_method
'\w scans, 71 frames at 1\% intervals, exposure time 2 minutes'
_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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.1891
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18505
_diffrn_reflns_theta_full        34.73
_diffrn_reflns_theta_max         34.73
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.681
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         8024
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.681
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                3556
_reflns_number_total             8024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31137b.txt
_cod_data_source_block           sja33_08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10129.9(13)
_cod_original_sg_symbol_H-M      R3C
_cod_database_code               7020263