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_7041406
_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 N7 O9 P3 Zn3'
_chemical_formula_weight         765.47
_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                62.121(12)
_cell_angle_beta                 76.294(19)
_cell_angle_gamma                88.84(2)
_cell_formula_units_Z            2
_cell_length_a                   8.621(5)
_cell_length_b                   15.529(8)
_cell_length_c                   16.001(7)
_cell_measurement_reflns_used    5158
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1829.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_method       'profile data from \w-scans'
_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  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1143
_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            19235
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-shape
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_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 167.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         0.677
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                6773
_reflns_number_total             8365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04363a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7041406--7041407.cif.'
_cod_original_cell_volume        1829.3(16)
_cod_database_code               7041406