Synthesis of ionisable [2 × 2] grid-type metallo-arrays and reversible protonic modulation of the optical properties of the [CoII4L4]8+ species
Ruben, Mario; Lehn, Jean-Marie; Vaughan, Gavin; Chemical Communications (Cambridge, United Kingdom)  (2003) 1338–1339; doi:10.1039/b303922f

data_7103717
_publ_section_title
;
 Synthesis of ionisable [2 \\times  2] grid-type metallo-arrays and
 reversible protonic modulation of the optical properties of the
 [CoII4L4]8+ species
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   12
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1338
_journal_page_last               1339
_journal_paper_doi               10.1039/b303922f
_journal_year                    2003
_chemical_formula_sum            'C100 H122 Cl8 Mn4 N44 O63'
_chemical_formula_weight         3451.78
_space_group_IT_number           2
_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                80.381(3)
_cell_angle_beta                 84.562(3)
_cell_angle_gamma                70.980(3)
_cell_formula_units_Z            2
_cell_length_a                   17.7576(12)
_cell_length_b                   17.9133(12)
_cell_length_c                   24.6470(15)
_cell_measurement_temperature    120(2)
_cell_volume                     7301.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.42753
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1113
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38752
_diffrn_reflns_theta_full        14.06
_diffrn_reflns_theta_max         14.06
_diffrn_reflns_theta_min         6.14
_exptl_absorpt_coefficient_mu    0.313
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3540
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2010
_refine_ls_number_reflns         19699
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.1155
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1048P)^2^+86.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2766
_refine_ls_wR_factor_ref         0.2902
_reflns_number_gt                14971
_reflns_number_total             19699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303922f.txt
_cod_data_source_block           mr250
_cod_database_code               7103717