Two hybrid transition metal triphosphonates decorated with a tripodal imidazole ligand: synthesis, structures and properties.
Wang, Guo-Ming; Li, Jin-Hua; Pan, Jie; Xue, Zhen-Zhen; Wei, Li; Han, Song-De; Bao, Zhen-Zhen; Wang, Zong-Hua; Dalton transactions (Cambridge, England : 2003) 46 (2017) 808–813; doi:10.1039/c6dt04363a

data_7041407
_publ_section_title
;
 Two hybrid transition metal triphosphonates decorated with a tripodal
 imidazole ligand: synthesis, structures and properties.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              808
_journal_page_last               813
_journal_paper_doi               10.1039/c6dt04363a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C18 H18 Co3 N7 O9 P3'
_chemical_formula_weight         746.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-10-04 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                62.066(13)
_cell_angle_beta                 76.251(17)
_cell_angle_gamma                88.765(19)
_cell_formula_units_Z            2
_cell_length_a                   8.645(4)
_cell_length_b                   15.658(7)
_cell_length_c                   15.977(6)
_cell_measurement_reflns_used    4341
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1845.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'XtaLABmini: Fixed Chi 2 circle'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19386
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-shape
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F^2^ was
written to a new HKL file. The number of located electrons, 
in one void per unit cell is 180.There are two formula units 
in one unit cell. On base of charge balance considerations, 
volume/count_electrons analysis, TG analyses and elemental analyses, 
this residual electron density was assigned to nine water molecules.  
So SQUEEZE removed these disordered units per unit cell. 
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                6344
_reflns_number_total             8420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04363a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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.

'_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7041406--7041407.cif.
;
_cod_database_code               7041407