Programmed Single Step Self-assembly of a [2x2] Grid Architecture Built on Metallic Centers of Different Coordination Geometries
Jean-Marie Lehn; Nathalie Kyritsakas; A. Petitjean; Chemical communications (Cambridge, England)  (2004) 1168–1169; doi:10.1039/b402854f

data_7102648
_publ_section_title
;
Programmed Single Step Self-assembly of a [2x2]
Grid Architecture Built on Metallic Centers of Different Coordination
Geometries
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1168
_journal_page_last               1169
_journal_paper_doi               10.1039/b402854f
_journal_year                    2004
_chemical_formula_moiety         'C238 H224 B3 Cu4 F15 N32 O18 S Zn4'
_chemical_formula_sum            'C238 H224 B3 Cu4 F15 N32 O18 S Zn4'
_chemical_formula_weight         4685.76
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                79.087(5)
_cell_angle_beta                 66.993(5)
_cell_angle_gamma                67.425(5)
_cell_formula_units_Z            1
_cell_length_a                   17.8009(3)
_cell_length_b                   18.2756(3)
_cell_length_c                   21.3141(4)
_cell_measurement_reflns_used    35951
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.4
_cell_volume                     5887.1(2)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
35951 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  1.4 deg 1 scans of  100 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  130 frames
Set 2 Theta =   -5.60 Kappa = -168.00 Phi   =    0.00   33 frames
Friedel pairs were averaged. Internal R = 0.06
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35951
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2422
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   10.909
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    70
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         11153
_refine_ls_number_restraints     -1
_refine_ls_R_factor_all          0.243
_refine_ls_R_factor_gt           0.105
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.661
_refine_ls_wR_factor_ref         0.137
_reflns_number_gt                11153
_reflns_number_total             26611
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b402854f.txt
_cod_data_source_block           st1293
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102648