Synthesis and structure of mononuclear and binuclear zinc(ii) compartmental macrocyclic complexes
Atkins, Andrew J.; Black, Daniel; Finn, Rachel L.; Marin-Becerra, Armando; Blake, Alexander J.; Ruiz-Ramirez, Lena; Li, Wan-Sheung; Schröder, Martin; Dalton Transactions  (2003) 1730–; doi:10.1039/b210936k

data_7012433
_publ_section_title
;
 Synthesis and structure of mononuclear and binuclear zinc(ii)
 compartmental macrocyclic complexes
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1730
_journal_paper_doi               10.1039/b210936k
_journal_year                    2003
_chemical_formula_moiety         'C28 H35 N5 O2 Zn 2+, 2(P F6 -)'
_chemical_formula_sum            'C28 H35 F12 N5 O2 P2 Zn'
_chemical_formula_weight         828.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   'difference map or placed geometrically'
_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                   15.34(2)
_cell_length_b                   19.998(7)
_cell_length_c                   21.537(12)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.0
_cell_measurement_theta_min      12.5
_cell_volume                     6607(10)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe, 1995)'
_computing_data_reduction        'X-RED (Stoe, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6612
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        9.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.546
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'X-RED (Stoe, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.54
_refine_diff_density_rms         0.10
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment
'methyl H atoms in rigid group, N-H with distance restraint; others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.049P)^2^+39.50P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.155
_refine_ls_wR_factor_ref         0.177
_reflns_number_gt                4633
_reflns_number_total             5804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210936k.txt
_cod_data_source_block           4
_cod_database_code               7012433