#------------------------------------------------------------------------------
#$Date: 2016-03-22 22:18:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179037 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/35/4123539.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4123539
loop_
_publ_author_name
'Kim, Yeong-Eun'
'Oh, Seohee'
'Kim, Seji'
'Kim, Onnuri'
'Kim, Jin'
'Han, Sang Woo'
'Lee, Yunho'
_publ_section_title
;
 Phosphinite-Ni(0) Mediated Formation of a Phosphide-Ni(II)-OCOOMe Species
 via Uncommon Metal-Ligand Cooperation.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4280
_journal_page_last               4283
_journal_paper_doi               10.1021/ja513112r
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C25 H39 I Ni P3, C H4 O, I'
_chemical_formula_sum            'C26 H43 I2 Ni O P3'
_chemical_formula_weight         777.02
_chemical_name_common            {(PPMeP)NiI}{I(MeOH)}
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.142(3)
_cell_length_b                   12.831(3)
_cell_length_c                   17.562(4)
_cell_measurement_reflns_used    45927
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.85
_cell_volume                     3186.7(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1088
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45927
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.8541
_exptl_absorpt_correction_T_min  0.7923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.901
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3407
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0747P)²+3.6534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                2573
_reflns_number_total             3407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja513112r_si_002.cif
_cod_data_source_block           0154a-2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

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

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 4123534--4123539.cif.
;
_cod_original_cell_volume        3186.8(11)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4123539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I -0.11395(4) 0.2500 0.28951(3) 0.02774(19) Uani 1 2 d SU
I2 I 0.69227(4) 0.7500 0.15746(3) 0.0302(2) Uani 1 2 d S
Ni1 Ni 0.02440(7) 0.2500 0.20298(5) 0.0189(2) Uani 1 2 d SU
O1 O 0.4513(5) 0.7500 0.0929(4) 0.0447(16) Uani 1 2 d SU
P1 P 0.10927(13) 0.2500 0.10300(11) 0.0210(4) Uani 1 2 d SU
P2 P 0.04908(9) 0.41906(11) 0.21010(8) 0.0211(3) Uani 1 1 d U
C1 C 0.0470(6) 0.2500 0.0114(5) 0.0282(17) Uani 1 2 d SU
H1A H 0.0932 0.2500 -0.0302 0.042 Uiso 1 2 calc SR
H1B H 0.0073 0.3124 0.0077 0.042 Uiso 0.50 1 calc PR
H1C H 0.0073 0.1876 0.0077 0.042 Uiso 0.50 1 calc PR
C2 C 0.1785(3) 0.3699(4) 0.0975(3) 0.0217(11) Uani 1 1 d U
C3 C 0.1492(4) 0.4482(4) 0.1471(3) 0.0215(11) Uani 1 1 d U
C4 C 0.1961(4) 0.5443(5) 0.1472(4) 0.0292(13) Uani 1 1 d U
H4A H 0.1768 0.5979 0.1811 0.035 Uiso 1 1 calc R
C5 C 0.2715(4) 0.5612(5) 0.0971(3) 0.0302(13) Uani 1 1 d U
H5A H 0.3046 0.6256 0.0981 0.036 Uiso 1 1 calc R
C6 C 0.2978(4) 0.4840(5) 0.0463(4) 0.0303(13) Uani 1 1 d U
H6A H 0.3478 0.4970 0.0114 0.036 Uiso 1 1 calc R
C7 C 0.2526(4) 0.3881(5) 0.0452(3) 0.0259(12) Uani 1 1 d U
H7A H 0.2711 0.3357 0.0101 0.031 Uiso 1 1 calc R
C8 C 0.1716(4) 0.4043(6) 0.3329(4) 0.0438(18) Uani 1 1 d U
H8A H 0.1930 0.4332 0.3816 0.066 Uiso 1 1 calc R
H8B H 0.2241 0.4044 0.2965 0.066 Uiso 1 1 calc R
H8C H 0.1495 0.3327 0.3406 0.066 Uiso 1 1 calc R
C9 C 0.0911(4) 0.4704(5) 0.3019(3) 0.0264(12) Uani 1 1 d U
H9A H 0.1181 0.5409 0.2913 0.032 Uiso 1 1 calc R
C10 C 0.0138(4) 0.4857(5) 0.3615(3) 0.0310(13) Uani 1 1 d U
H10A H 0.0419 0.5131 0.4084 0.047 Uiso 1 1 calc R
H10B H -0.0167 0.4186 0.3721 0.047 Uiso 1 1 calc R
H10C H -0.0333 0.5350 0.3422 0.047 Uiso 1 1 calc R
C11 C -0.0312(4) 0.6197(5) 0.1861(4) 0.0383(15) Uani 1 1 d U
H11A H -0.0879 0.6583 0.1708 0.057 Uiso 1 1 calc R
H11B H 0.0211 0.6370 0.1516 0.057 Uiso 1 1 calc R
H11C H -0.0139 0.6387 0.2383 0.057 Uiso 1 1 calc R
C12 C -0.0511(4) 0.5027(4) 0.1820(3) 0.0254(12) Uani 1 1 d U
H12A H -0.1038 0.4881 0.2184 0.030 Uiso 1 1 calc R
C13 C -0.0860(4) 0.4720(5) 0.1027(3) 0.0333(14) Uani 1 1 d U
H13A H -0.1396 0.5163 0.0884 0.050 Uiso 1 1 calc R
H13B H -0.1060 0.3989 0.1031 0.050 Uiso 1 1 calc R
H13C H -0.0347 0.4812 0.0657 0.050 Uiso 1 1 calc R
C14 C 0.4723(8) 0.7500 0.0147(6) 0.059(3) Uani 1 2 d SU
H14A H 0.4873 0.8211 -0.0018 0.089 Uiso 0.50 1 calc PR
H14B H 0.4174 0.7244 -0.0139 0.089 Uiso 0.50 1 calc PR
H14C H 0.5267 0.7045 0.0051 0.089 Uiso 0.50 1 calc PR
H1 H 0.523(8) 0.7500 0.115(6) 0.07(3) Uiso 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Ni1 P2 87.56(4) . 7_565
P1 Ni1 P2 87.56(4) . .
P2 Ni1 P2 160.60(8) 7_565 .
P1 Ni1 I1 162.19(7) . .
P2 Ni1 I1 95.19(4) 7_565 .
P2 Ni1 I1 95.19(4) . .
H1 O1 C14 99(6) . .
C2 P1 C2 114.8(3) . 7_565
C2 P1 C1 102.2(2) . .
C2 P1 C1 102.2(2) 7_565 .
C2 P1 Ni1 110.27(18) . .
C2 P1 Ni1 110.27(18) 7_565 .
C1 P1 Ni1 117.0(3) . .
C3 P2 C9 101.9(2) . .
C3 P2 C12 108.2(2) . .
C9 P2 C12 105.9(3) . .
C3 P2 Ni1 106.80(18) . .
C9 P2 Ni1 117.0(2) . .
C12 P2 Ni1 115.91(18) . .
C3 C2 C7 120.5(5) . .
C3 C2 P1 114.5(4) . .
C7 C2 P1 124.9(4) . .
C2 C3 C4 119.7(5) . .
C2 C3 P2 117.4(4) . .
C4 C3 P2 123.0(4) . .
C5 C4 C3 119.8(6) . .
C6 C5 C4 120.0(5) . .
C5 C6 C7 121.3(5) . .
C6 C7 C2 118.7(5) . .
C8 C9 C10 111.2(5) . .
C8 C9 P2 110.9(4) . .
C10 C9 P2 114.6(4) . .
C11 C12 C13 110.8(5) . .
C11 C12 P2 114.7(4) . .
C13 C12 P2 110.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Ni1 2.4774(11) .
Ni1 P1 2.127(2) .
Ni1 P2 2.2006(15) 7_565
Ni1 P2 2.2006(15) .
O1 H1 1.08(11) .
O1 C14 1.405(12) .
P1 C2 1.826(6) .
P1 C2 1.826(6) 7_565
P1 C1 1.834(8) .
P2 C3 1.836(5) .
P2 C9 1.839(6) .
P2 C12 1.844(5) .
C2 C3 1.393(7) .
C2 C7 1.412(7) .
C3 C4 1.400(8) .
C4 C5 1.399(8) .
C5 C6 1.386(9) .
C6 C7 1.387(8) .
C8 C9 1.521(8) .
C9 C10 1.526(8) .
C11 C12 1.528(8) .
C12 C13 1.530(8) .
