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_7214346
_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         '2(C40 H44 Cl N4 Ni O8), Cl4 Ni'
_chemical_formula_sum            'C80 H88 Cl6 N8 Ni3 O16'
_chemical_formula_weight         1806.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-27
_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                   16.298(2)
_cell_length_b                   16.298(2)
_cell_length_c                   30.945(6)
_cell_measurement_temperature    100(2)
_cell_volume                     8220(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            69812
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.41
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Multi-scan absorption correction within XDS suite'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3752
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4959
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+27.8654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                4394
_reflns_number_total             4959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42141d.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7214346
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H21A,H21B} of C21, {H10A,H10B} of C10, {H11A,H11B} of C11,
   {H6A,H6B} of C6, {H9A,H9B} of C9, {H7A,H7B} of C7
 At 1.5 times of:
  {H20,H30} of C13
2. Restrained distances
 H20-O20
 0.84 with sigma of 0.02
 H30-O30
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C6(H6A,H6B),
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C17(H17), C14(H14), C24(H24), C26(H26), C27(H27), C13(H13)
;