Assembling metal phosphonates in the presence of monodentate-terminal and bidentate-bridging pyridine ligands. Use of non-covalent and covalent-coordinate interactions to build polymeric metal–phosphonate architectures
Murugavel, Ramaswamy; Shanmugan, Swaminathan; Dalton Transactions  (2008) 5358–5367; doi:10.1039/b805848b

data_7004338
_publ_section_title
;
 Assembling metal phosphonates in the presence of monodentate-terminal
 and bidentate-bridging pyridine ligands. Use of non-covalent and
 covalent-coordinate interactions to build polymeric metal--phosphonate
 architectures
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              5358
_journal_page_last               5367
_journal_paper_doi               10.1039/b805848b
_journal_year                    2008
_chemical_formula_moiety         'C36 H60 Co4 N8 O12 P4'
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_cell_length_a                   20.1451(4)
_cell_length_b                   20.1451(4)
_cell_length_c                   12.7796(5)
_cell_measurement_reflns_used    4555
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_cell_volume                     5186.3(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -101.00 -51.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -29.0346 -45.0000 120.0000 0.0000 0.0000 50

2 omega -61.00 -7.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -29.0346 75.0000 120.0000 0.0000 0.0000 54

3 omega -53.00 -2.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -29.0346 -45.0000 120.0000 0.0000 0.0000 51

4 omega 43.00 91.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -127.0000 281.0000 0.0000 0.0000 48

5 omega -2.00 51.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 75.0000 240.0000 0.0000 0.0000 53

6 omega 6.00 57.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -45.0000 240.0000 0.0000 0.0000 51

7 omega -2.00 43.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -127.0000 281.0000 0.0000 0.0000 45

8 omega -43.00 9.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -45.0000 0.0000 0.0000 0.0000 52

9 omega 9.00 51.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -75.0000 0.0000 0.0000 0.0000 42

10 phi 49.00 91.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 29.5033 0.0000 - 0.0000 0.0000 42

11 omega 51.00 102.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 45.0000 0.0000 0.0000 0.0000 51

12 omega -43.00 7.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 29.5033 -45.0000 240.0000 0.0000 0.0000 50

13 phi 118.00 180.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 29.5033 0.0000 - 0.0000 0.0000 62

;
_diffrn_measurement_device_type  'OXFORD DIFFRACTIOM X CALIBUR-S'
_diffrn_measurement_method       'omega(w)-q scan'
_diffrn_orient_matrix_UB_11      0.0145705477
_diffrn_orient_matrix_UB_12      0.0018143318
_diffrn_orient_matrix_UB_13      -0.0504655803
_diffrn_orient_matrix_UB_21      -0.0319513163
_diffrn_orient_matrix_UB_22      0.0036067010
_diffrn_orient_matrix_UB_23      -0.0225859921
_diffrn_orient_matrix_UB_31      0.0025512040
_diffrn_orient_matrix_UB_32      0.0349879227
_diffrn_orient_matrix_UB_33      0.0049119904
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25032
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.7615
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                1586
_reflns_number_total             2288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805848b.txt
_cod_data_source_block           newrm161-relable
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7004338