Preparation and solid-state characterization of nickel(II) complexes with 1'-(diphenylphosphino)ferrocenecarboxylic acid
Pinkas, Jiří; Bastl, Zdeněk; Šlouf, Miroslav; Podlaha, Jaroslav; Štěpnička, Petr; New Journal of Chemistry 25 (2001) 1215–; doi:10.1039/b104780a

data_7051194
_publ_section_title
;
 Preparation and solid-state characterization of nickel(II) complexes
 with 1'-(diphenylphosphino)ferrocenecarboxylic acid
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1215
_journal_paper_doi               10.1039/b104780a
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         '[Ni(C23H19PO2Fe)2(NCS)2] * 2CHCl3'
_chemical_formula_sum            'C50 H40 Cl6 Fe2 N2 Ni O4 P2 S2'
_chemical_formula_weight         1242.01
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.832(5)
_cell_angle_beta                 73.892(4)
_cell_angle_gamma                71.608(4)
_cell_formula_units_Z            1
_cell_length_a                   10.724(1)
_cell_length_b                   11.0215(6)
_cell_length_c                   12.758(1)
_cell_measurement_reflns_used    5956
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     1344.24(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      296(1)
_diffrn_detector_area_resol_mean 0.110
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
CCD
(rotation scans, rotation per image 2\%, exposure per frame 120 s,
108 images collected using 168\% \f and 48\% \w scans, 
which corresponds to the half of Ewald sphere)
;
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10558
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0890P)^2^+0.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                2929
_reflns_number_total             4744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104780a.txt
_cod_data_source_block           niscn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1344.2(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051194