Autoionization of Homogeneous Nickel(II) Diphosphane Hydrogenation Catalysts. An NMR Study and Crystal Structures of [Ni(o-MeO-dppe)I2] and [Ni(o-MeO-dppe)2](PF6)2
Ingrid M. Angulo; Elisabeth Bouwman; Martin Lutz; Wilhelmus P. Mul; Anthony L. Spek; Inorganic Chemistry 40 (2001) 2073–2082; doi:10.1021/ic0006955

data_4319529
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Dep. Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Autoionization of Homogeneous Nickel(II) Diphosphane Hydrogenation
 Catalysts. An NMR Study and Crystal Structures of [Ni(o-MeO-dppe)I2] and
 [Ni(o-MeO-dppe)2](PF6)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2073
_journal_page_last               2082
_journal_paper_doi               10.1021/ic0006955
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C30 H32 I2 Ni O4 P2'
_chemical_formula_sum            'C30 H32 I2 Ni O4 P2'
_chemical_formula_weight         831.01
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.3250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1309(1)
_cell_length_b                   16.5759(3)
_cell_length_c                   17.6474(2)
_cell_measurement_temperature    150(2)
_cell_volume                     3093.82(8)
_computing_cell_refinement       'DENZO 1.11.0'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO 1.11.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47807
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.441
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.6536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                6084
_reflns_number_total             7113
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0006955_2.cif
_cod_data_source_block           s1917c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3093.82(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4319529