Unexpected metal ion-assisted transformations leading to unexplored bridging ligands in Ni(II) coordination chemistry: the case of PO3F(2-) group.
Dermitzaki, Despina; Raptopoulou, Catherine P.; Psycharis, Vassilis; Escuer, Albert; Perlepes, Spyros P.; Stamatatos, Theocharis C.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14520–14524; doi:10.1039/c4dt02204a

data_7032024
_publ_section_title
;
 Unexpected metal ion-assisted transformations leading to unexplored
 bridging ligands in Ni(II) coordination chemistry: the case of PO3F(2-)
 group.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14520
_journal_page_last               14524
_journal_paper_doi               10.1039/c4dt02204a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C43.35 H56.4 F14 N12 Ni3 O14.85 P4'
_chemical_formula_weight         1549.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.689(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3467(3)
_cell_length_b                   17.1048(3)
_cell_length_c                   24.5607(4)
_cell_measurement_reflns_used    44485
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      71.85
_cell_measurement_theta_min      6.51
_cell_volume                     6942.9(2)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52382
_diffrn_reflns_theta_full        61.00
_diffrn_reflns_theta_max         61.00
_diffrn_reflns_theta_min         6.97
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3157
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         10461
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1759P)^2^+3.7507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2621
_reflns_number_gt                7720
_reflns_number_total             10461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02204a2.cif
_cod_data_source_block           comp1
_cod_depositor_comments
'Adding full bibliography for 7032024--7032027.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C43.35 H56.40 F14 N12 Ni3 O14.85 P4'
_cod_database_code               7032024