Self-sorting of metallosupramolecular DCLs via double-level exchange: amplification in solution and solid state modulation.
Dumitru, Florina; Legrand, Yves-Marie; Petit, Eddy; van der Lee, Arie; Barboiu, Mihail; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11860–11865; doi:10.1039/c2dt31532g

data_7030135
_publ_section_title
;
 Self-sorting of metallosupramolecular DCLs via double-level exchange:
 amplification in solution and solid state modulation.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11860
_journal_page_last               11865
_journal_paper_doi               10.1039/c2dt31532g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'C38 H28.64 N6 O2.64 Zn, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H34.64 F6 N8 O8.64 S2 Zn'
_chemical_formula_weight         1057.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 113.340(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4340(16)
_cell_length_b                   8.3120(5)
_cell_length_c                   23.7330(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4606.8(5)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.50915
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68831
_diffrn_reflns_theta_full        20.867
_diffrn_reflns_theta_max         21.292
_diffrn_reflns_theta_min         0.625
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2158.953
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.83
_refine_diff_density_min         -1.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0501
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         11254
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.0047480
_refine_ls_shift/su_mean         0.0000505
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.519 0.538 0.285
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0477
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0401
_reflns_limit_h_max              33
_reflns_limit_h_min              -36
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                11254
_reflns_number_total             13674
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0451
_oxford_refine_ls_scale          0.17974(18)
_oxford_reflns_number_all        13656
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c2dt31532g.txt
_cod_data_source_block           1_mdbm37
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7030135
_montpellier_reflns_maxres       0.701
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S, H(341,X'S), H(101,X'S), H(471,X'S)
CONT H(231,X'S)
EQUIV O(47,OCC) UNTIL H(471)
EQUIV O(34,OCC) UNTIL H(341)
EQUIV O(23,OCC) UNTIL H(231)
EQUIV O(10,OCC) UNTIL H(101)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 68,X'S) H ( 681,X'S) H ( 682,X'S) H ( 683,X'S)
RIDE C ( 71,X'S) H ( 711,X'S) H ( 712,X'S) H ( 713,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
A-U(IJ)'S 0.00,0.001 = C(46) TO O(47), C(33) TO O(34), C(9) TO O(10),
CONT C(22) TO O(23)
ANGLE 109.5, 0.3 = H(341) TO O(34) TO C(33)
ANGLE 109.5, 0.3 = H(101) TO O(10) TO C(9)
ANGLE 109.5, 0.3 = H(471) TO O(47) TO C(46)
ANGLE 109.5, 0.3 = H(231) TO O(23) TO C(22)
DIST 0.82, 0.01 = H(341) TO O(34)
DIST 0.82, 0.01 = H(101) TO O(10)
DIST 0.82, 0.01 = H(471) TO O(47)
DIST 0.82, 0.01 = H(231) TO O(23)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;