Two distinct tetranuclear motifs, rectangular vs. extended, are observed for complexes of a bis-tetradentate pyrimidine-based ligand
Gobeze, Worku A.; Brooker, Sally; RSC Advances 3 (2013) 24307–; doi:10.1039/c3ra45091k

data_7239350
_publ_section_title
;
 Two distinct tetranuclear motifs, rectangular vs. extended, are observed
 for complexes of a bis-tetradentate pyrimidine-based ligand
;
_journal_issue                   46
_journal_name_full               'RSC Advances'
_journal_page_first              24307
_journal_paper_doi               10.1039/c3ra45091k
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C73 H79 Cl8 Cu4 N16 O4.5'
_chemical_formula_weight         1790.28
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                118.696(8)
_cell_angle_beta                 99.214(12)
_cell_angle_gamma                98.490(12)
_cell_formula_units_Z            1
_cell_length_a                   12.727(4)
_cell_length_b                   13.733(2)
_cell_length_c                   13.977(2)
_cell_measurement_reflns_used    7037
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.71
_cell_volume                     2042.9(8)
_computing_cell_refinement       'APEX2 & SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Kappa Apex II area detector'
_diffrn_measurement_method       '\f and \w 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42552
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  0.8772
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             917
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.912
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8310
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+6.9150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                7025
_reflns_number_total             8310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra45091k.txt
_cod_data_source_block           wag345
_cod_original_cell_volume        2042.8(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C73 H79 Cl8 Cu4 N16 O4.50'
_cod_database_code               7239350