Synthesis, structure, and electrochemistry of di- and zerovalent nickel, palladium, and platinum monomers and dimers derived from an enantiopure (S,S)-tetra(tertiary phosphine).
Kitto, Heather J.; Rae, A. David; Webster, Richard D.; Willis, Anthony C.; Wild, S. Bruce; Inorganic chemistry 46 (2007) 8059–8070; doi:10.1021/ic700912q

data_4339829
_publ_section_title
;
 Synthesis, structure, and electrochemistry of di- and zerovalent nickel,
 palladium, and platinum monomers and dimers derived from an enantiopure
 (S,S)-tetra(tertiary phosphine).
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8059
_journal_page_last               8070
_journal_paper_doi               10.1021/ic700912q
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C44 H45 N Ni P4 2+, (C F3 O3 S -)2 '
_chemical_formula_sum            'C46 H45 F6 N Ni O6 P4 S2'
_chemical_formula_weight         1068.59
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-15-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-02-16 - Report on C46 H45 F6 N Ni O6 P4 S2
             by Anthony C. Willis
             for   Heather J. Kitto and S. Bruce Wild

2005-02-16 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2784(1)
_cell_length_b                   19.3240(2)
_cell_length_c                   37.3338(4)
_cell_measurement_reflns_used    112592
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     9579.55(16)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            92042
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.607
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.13
_refine_ls_abs_structure_details 'Flack, 7650 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1872
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         11403
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.022
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.812 0.317 0.561 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0567
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0463
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                11403
_reflns_number_total             16875
_reflns_threshold_expression     I>3.0u(I)
_cod_data_source_file            ic700912q-file001.cif
_cod_data_source_block           1_hjk6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C46 H45 F6 N Ni O6 P4 S2 '
_cod_database_code               4339829