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_7030136
_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 H30 N6 O4 Zn, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H36 F6 N8 O10 S2 Zn'
_chemical_formula_weight         1080.34
_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     other
_cell_angle_alpha                90
_cell_angle_beta                 113.144(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5485(11)
_cell_length_b                   8.2860(3)
_cell_length_c                   23.8465(11)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    175
_cell_measurement_theta_max      32.4240
_cell_measurement_theta_min      2.8736
_cell_volume                     4641.9(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
1 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 0.0000 115

2 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 90.0000 115

3 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 180.0000 115

4 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 270.0000 115

5 omega -111.00 10.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -80.0000 100.0000 121

6 omega -116.00 71.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -10.0000 180.0000 187

7 omega -110.00 12.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -80.0000 0.0000 122

;
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0272925000
_diffrn_orient_matrix_UB_12      -0.0273244000
_diffrn_orient_matrix_UB_13      0.0030431000
_diffrn_orient_matrix_UB_21      -0.0064470000
_diffrn_orient_matrix_UB_22      0.0203637000
_diffrn_orient_matrix_UB_23      -0.0308928000
_diffrn_orient_matrix_UB_31      0.0111832000
_diffrn_orient_matrix_UB_32      0.0785490000
_diffrn_orient_matrix_UB_33      0.0090758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.140
_diffrn_reflns_av_sigmaI/netI    0.3193
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            87153
_diffrn_reflns_theta_full        27.623
_diffrn_reflns_theta_max         32.497
_diffrn_reflns_theta_min         2.879
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.46
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         7541
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.0011638
_refine_ls_shift/su_mean         0.0000312
_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:
3.04 -3.87 1.72 -0.742 -0.687
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0975
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0507
_reflns_limit_h_max              35
_reflns_limit_h_min              -38
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                7541
_reflns_number_total             15280
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.17
_oxford_diffrn_Wilson_scale      5.15
_oxford_refine_ls_r_factor_ref   0.0720
_oxford_refine_ls_scale          0.4089(5)
_oxford_reflns_number_all        15280
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c2dt31532g.txt
_cod_data_source_block           1_vdlee46
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7030136
_cell_oxdiff_length_a            23.8501(9)
_cell_oxdiff_length_b            8.2840(3)
_cell_oxdiff_length_c            25.5491(9)
_cell_oxdiff_angle_alpha         89.972(3)
_cell_oxdiff_angle_beta          113.140(3)
_cell_oxdiff_angle_gamma         89.998(3)
_cell_oxdiff_volume              4641.7(3)
_cell_oxdiff_measurement_reflns_used 9410
_montpellier_reflns_maxres       0.81
_montpellier_reflns_completeness_maxres 99.78
_montpellier_reflns_redundancy_maxres 7.07
_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)
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)
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
;