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_7032027
_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            'C15.2 H19.1 F2 N4.6 Ni O7.65 P2'
_chemical_formula_weight         547.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 111.294(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9266(6)
_cell_length_b                   18.0040(11)
_cell_length_c                   13.3621(8)
_cell_measurement_reflns_used    7966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.01
_cell_measurement_theta_min      6.51
_cell_volume                     2673.3(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0891
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10864
_diffrn_reflns_theta_full        52.00
_diffrn_reflns_theta_max         52.00
_diffrn_reflns_theta_min         6.70
_exptl_absorpt_coefficient_mu    2.696
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1119
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0007(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.1065
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2618
_refine_ls_wR_factor_ref         0.3231
_reflns_number_gt                1356
_reflns_number_total             2728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02204a2.cif
_cod_data_source_block           comp4
_cod_depositor_comments
'Adding full bibliography for 7032024--7032027.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C15.20 H19.10 F2 N4.60 Ni O7.65 P2'
_cod_database_code               7032027