Transition Metal Complexes of Phosphinous Acids Featuring a Quasichelating Unit: Synthesis, Characterization, and Hetero-bimetallic Complexes.
Allefeld, Nadine; Bader, Julia; Neumann, Beate; Stammler, Hans-Georg; Ignat'ev, Nikolai; Hoge, Berthold; Inorganic chemistry 54 (2015) 7945–7952; doi:10.1021/acs.inorgchem.5b01038

data_4346238
_publ_section_title
;
 Transition Metal Complexes of Phosphinous Acids Featuring a
 Quasichelating Unit: Synthesis, Characterization, and Hetero-bimetallic
 Complexes.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7945
_journal_page_last               7952
_journal_paper_doi               10.1021/acs.inorgchem.5b01038
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C36 H44 F24 Ni4 O14 P4'
_chemical_formula_sum            'C36 H44 F24 Ni4 O14 P4'
_chemical_formula_weight         1515.43
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                100.628(2)
_cell_angle_beta                 103.287(2)
_cell_angle_gamma                100.273(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1196(6)
_cell_length_b                   9.4568(6)
_cell_length_c                   17.0109(11)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.486
_cell_measurement_theta_min      2.746
_cell_volume                     1365.42(15)
_computing_cell_refinement       'APEX 2, Bruker AXS'
_computing_data_collection       'APEX 2, Bruker AXS'
_computing_data_reduction        'APEX 2, Bruker AXS'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector Ultra with APEX II'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'Quazar Montel multilayer optic Montel200'
_diffrn_radiation_source         'I\mS Incoatec Microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18049
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.99
_diffrn_reflns_theta_min         4.89
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.7774
_exptl_absorpt_correction_T_min  0.5393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0782P)^2^+0.9418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                4725
_reflns_number_total             5030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01038_si_004.cif
_cod_data_source_block
'[{(acac)Ni[P(CF~3~)~2~O]~2~}~2~Ni~2~(acac)~2~].2THF'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4346238