Self-assembly of discrete and polymeric metallosupramolecular architectures from cyclen-derived ligands
Hawes, Chris S.; Batten, Stuart R.; Turner, David R.; CrystEngComm 16 (2014) 3737–; doi:10.1039/c3ce42141d

data_7214348
_publ_section_title
;
 Self-assembly of discrete and polymeric metallosupramolecular
 architectures from cyclen-derived ligands
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3737
_journal_paper_doi               10.1039/c3ce42141d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'0.5(C168 H192 Cl4 Cu8 N16 O36), 0.25(Cl16 Cu4), 5(H2O)'
_chemical_formula_sum            'C84 H106 Cl6 Cu5 N8 O23'
_chemical_formula_weight         2126.17
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.258(5)
_cell_length_b                   8.7597(15)
_cell_length_c                   29.409(4)
_cell_measurement_reflns_used    2017
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.261
_cell_measurement_theta_min      2.396
_cell_volume                     9083(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            30080
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0737 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.9153.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4388
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+57.9423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2311
_reflns_number_gt                3347
_reflns_number_total             5579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42141d.txt
_cod_data_source_block           4
_cod_database_code               7214348
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H40A,H40B} of C40, {H10A,H10B} of C10, {H13A,H13B} of C13,
   {H11A,H11B} of C11, {H14A,H14B} of C14, {H18A,H18B} of C18, {H2A,H2B} of C2,
  {H19A,H19B} of C19, {H16A,H16B} of C16, All N(H,H,H,H,H) groups
 At 1.5 times of:
  {H41A,H41B} of C40
2. Restrained distances
 C9-H9A
 0.99 with sigma of 0.02
 C9-H9B
 0.99 with sigma of 0.02
 C20-H20B
 0.99 with sigma of 0.02
 C20-H20A
 0.99 with sigma of 0.02
 H37-O37
 0.84 with sigma of 0.02
 H41A_$2-H41A
 1.6 with sigma of 0.02
 H41A_$2-H41B
 1.6 with sigma of 0.02
 H41B-H41A
 1.6 with sigma of 0.02
 H41A_$2-C41
 0.99 with sigma of 0.02
 H41A-C41
 0.99 with sigma of 0.02
 H41B-C41
 0.99 with sigma of 0.02
 H41B-C40
 2 with sigma of 0.02
 H41A_$2-C40
 2 with sigma of 0.02
 H41A-C40_$2
 2 with sigma of 0.02
 H40-O39
 0.84 with sigma of 0.02
 O40-H40
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N17) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
4. Others
 Fixed Sof: Cu3(0.25) Cl7(0.25) Cl8(0.25) O40(0.16667) C13(0.5) H13A(0.5)
 H13B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C14(0.5)
 H14A(0.5) H14B(0.5) C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) Cl5(0.25) Cl6(0.25) C10(0.5) H10A(0.5) H10B(0.5)
 N12(0.5) N15(0.5) N17(0.5) N9(0.5) O44(0.41666) O43(0.83333) O39(0.3333)
 C40(0.5) H40A(0.5) H40B(0.5) H40(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C11(H11A,H11B), C2(H2A,H2B), C14(H14A,H14B), C18(H18A,H18B),
 C19(H19A,H19B), C16(H16A,H16B), C10(H10A,H10B), C40(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C34(H34), C22(H22), C32(H32), C31(H31), C26(H26), C25(H25), C23(H23)
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