Catenation control in the two-dimensional coordination polymers based on tritopic carboxylate linkers and azamacrocyclic nickel(ii) complexes.
Lampeka, Yaroslaw D.; Tsymbal, Liudmyla V.; Barna, Andrij V.; Shuĺga, Yulija L; Shova, Sergiu; Arion, Vladimir B.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 4118–4125; doi:10.1039/c2dt11980c

data_7018427
_publ_section_title
;
 Catenation control in the two-dimensional coordination polymers based on
 tritopic carboxylate linkers and azamacrocyclic nickel(ii) complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4118
_journal_page_last               4125
_journal_paper_doi               10.1039/c2dt11980c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         '2n(C42 H51 N6 Ni1.5 O6), 6n(H2 O)'
_chemical_formula_sum            'C84 H114 N12 Ni3 O18'
_chemical_formula_weight         1756.00
_chemical_name_common
;
catena-(bis(mu!3$(4,4',4''-benzene-1,3,5-triyl-tribenzoato)-
O,O',O'') -tris((1,4,8,11-tetra-azacyclotetradecane)-nickel(ii))
hexahydrate)
;
_chemical_name_systematic
;
catena-(bis(\m~3~(4,4',4''-benzene-1,3,5-triyl-tribenzoato)-O,O',O'')
-tris((1,4,8,11-tetra-azacyclotetradecane)-nickel(ii)) hexahydrate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1953(15)
_cell_length_b                   20.339(3)
_cell_length_c                   29.599(5)
_cell_measurement_reflns_used    893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8117
_cell_measurement_theta_min      2.8611
_cell_volume                     4317.3(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9914
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
1 omega -52.00 67.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 20.4664 0.0000 150.0000 119

2 omega -26.00 -1.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 20.4664 104.0000 -104.0000 25

3 omega 7.00 85.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 20.4664 37.0000 0.0000 78

4 omega 60.00 100.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 20.4664 179.0000 150.0000 40

5 omega 60.00 93.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 20.4664 179.0000 -30.0000 33

6 omega -18.00 15.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- -21.2476 -104.0000 -25.0000 33

7 omega -104.00 -32.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- -21.2476 179.0000 30.0000 72
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0391750000
_diffrn_orient_matrix_UB_12      -0.0041397000
_diffrn_orient_matrix_UB_13      0.0209992000
_diffrn_orient_matrix_UB_21      0.0863982000
_diffrn_orient_matrix_UB_22      -0.0123401000
_diffrn_orient_matrix_UB_23      0.0097348000
_diffrn_orient_matrix_UB_31      0.0279785000
_diffrn_orient_matrix_UB_32      0.0323234000
_diffrn_orient_matrix_UB_33      0.0064049000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1134
_diffrn_reflns_av_unetI/netI     0.2256
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            20298
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.3022
_refine_ls_R_factor_gt           0.0852
_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
[0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0100P)^2^+0.0000sin\q/\l]
where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1948
_reflns_number_gt                2330
_reflns_number_total             7536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11980c.txt
_cod_data_source_block           NiL1_BTB
_cod_original_cell_volume        4317.3(14)
_cod_database_code               7018427
_chemical_oxdiff_formula         C31H30N4O6Ni1
_reflns_odcompleteness_completeness 74.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32