#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:14:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178641 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/52/4075277.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_4075277
loop_
_publ_author_name
'Rufińska, Anna'
'Goddard, Richard'
'Weidenthaler, Claudia'
'Bühl, Michael'
'Pörschke, Klaus-Richard'
_publ_section_title
;
 Structural Properties and Dynamics of Five-Coordinate
 Nickel(II)−π-Allyl Complexes Containing Monodentate Phosphorus
 Ligands
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2308
_journal_paper_doi               10.1021/om0601807
_journal_volume                  25
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_compound_source        dichloromethane/diethylether
_chemical_formula_moiety         'C12 H32 Ni O9 P3 1+, Br 1-'
_chemical_formula_sum            'C12 H32 Br Ni O9 P3'
_chemical_formula_weight         551.91
_chemical_name_systematic
; 
 η³-allyl-trimethylphosphite-nickel(ii)-bromide  
;
_chemical_temperature_decomposition_gt 333
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.078(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7181(2)
_cell_length_b                   8.1124(1)
_cell_length_c                   12.6683(2)
_cell_measurement_reflns_used    32422
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.91
_cell_volume                     1095.31(3)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD ω-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27294
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.967
_exptl_absorpt_correction_T_max  0.75063
_exptl_absorpt_correction_T_min  0.63256
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(8)
_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     235
_refine_ls_number_reflns         6968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0496
_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/[σ²(Fo²)+(0.0141P)²+1.1830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                5606
_reflns_number_total             6968
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0601807si20060223_123426.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '>333
decomposition' was changed to '333' - it should be numeric and
without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_database_code               4075277
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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
C1 C 0.7159(4) -0.1694(6) 0.8916(4) 0.0246(10) Uani 1 1 d .
H1A H 0.6624 -0.1118 0.9366 0.030 Uiso 1 1 calc R
H1B H 0.6857 -0.2781 0.8695 0.030 Uiso 1 1 calc R
C2 C 0.8444(4) -0.1508(6) 0.9154(3) 0.0219(9) Uani 1 1 d .
H2 H 0.8808 -0.0954 0.9802 0.026 Uiso 1 1 calc R
C3 C 0.9183(4) -0.2167(5) 0.8423(3) 0.0208(9) Uani 1 1 d .
H3A H 0.8988 -0.3279 0.8176 0.025 Uiso 1 1 calc R
H3B H 1.0073 -0.1923 0.8525 0.025 Uiso 1 1 calc R
C4 C 1.0590(4) -0.1468(5) 0.6249(4) 0.0209(9) Uani 1 1 d .
H4A H 1.0960 -0.1686 0.5606 0.031 Uiso 1 1 calc R
H4B H 0.9862 -0.2151 0.6275 0.031 Uiso 1 1 calc R
H4C H 1.1187 -0.1706 0.6849 0.031 Uiso 1 1 calc R
C5 C 1.0220(4) 0.3902(5) 0.6554(4) 0.0232(10) Uani 1 1 d .
H5A H 0.9823 0.4913 0.6310 0.035 Uiso 1 1 calc R
H5B H 1.0654 0.3437 0.5999 0.035 Uiso 1 1 calc R
H5C H 1.0808 0.4119 0.7163 0.035 Uiso 1 1 calc R
C6 C 1.2021(4) 0.1341(6) 0.8083(4) 0.0261(10) Uani 1 1 d .
H6A H 1.2494 0.1353 0.8770 0.039 Uiso 1 1 calc R
H6B H 1.2118 0.2379 0.7736 0.039 Uiso 1 1 calc R
H6C H 1.2322 0.0470 0.7663 0.039 Uiso 1 1 calc R
C7 C 0.5109(4) 0.3624(6) 0.6882(4) 0.0261(10) Uani 1 1 d .
H7A H 0.4791 0.3790 0.6152 0.039 Uiso 1 1 calc R
H7B H 0.5412 0.4651 0.7185 0.039 Uiso 1 1 calc R
H7C H 0.4449 0.3214 0.7267 0.039 Uiso 1 1 calc R
C8 C 0.5261(4) 0.2811(7) 0.9448(4) 0.0293(11) Uani 1 1 d .
H8A H 0.4657 0.2299 0.9851 0.044 Uiso 1 1 calc R
H8B H 0.4853 0.3629 0.8986 0.044 Uiso 1 1 calc R
H8C H 0.5904 0.3324 0.9923 0.044 Uiso 1 1 calc R
C9 C 0.8405(4) 0.3604(6) 0.9353(3) 0.0197(9) Uani 1 1 d .
H9A H 0.8691 0.4709 0.9504 0.029 Uiso 1 1 calc R
H9B H 0.9101 0.2927 0.9207 0.029 Uiso 1 1 calc R
H9C H 0.8039 0.3169 0.9954 0.029 Uiso 1 1 calc R
C10 C 0.4708(4) -0.1445(6) 0.6877(3) 0.0205(9) Uani 1 1 d .
H10A H 0.3855 -0.1380 0.6561 0.031 Uiso 1 1 calc R
H10B H 0.4877 -0.0544 0.7363 0.031 Uiso 1 1 calc R
H10C H 0.4835 -0.2469 0.7253 0.031 Uiso 1 1 calc R
C11 C 0.7206(4) 0.0747(5) 0.4825(3) 0.0198(9) Uani 1 1 d .
H11A H 0.7476 0.0868 0.4130 0.030 Uiso 1 1 calc R
H11B H 0.7672 0.1490 0.5308 0.030 Uiso 1 1 calc R
H11C H 0.6328 0.0997 0.4796 0.030 Uiso 1 1 calc R
C12 C 0.7048(4) -0.4346(5) 0.5369(3) 0.0225(10) Uani 1 1 d .
H12A H 0.7330 -0.5457 0.5503 0.034 Uiso 1 1 calc R
H12B H 0.7438 -0.3903 0.4783 0.034 Uiso 1 1 calc R
H12C H 0.6153 -0.4339 0.5202 0.034 Uiso 1 1 calc R
Br1 Br 0.26499(4) 0.60525(5) 0.83476(3) 0.01991(10) Uani 1 1 d .
Ni1 Ni 0.79895(4) -0.02845(6) 0.77992(4) 0.01200(11) Uani 1 1 d .
O1 O 1.0229(3) 0.0236(3) 0.6275(2) 0.0157(6) Uani 1 1 d .
O2 O 0.9283(2) 0.2757(3) 0.6837(2) 0.0173(6) Uani 1 1 d .
O3 O 1.0703(2) 0.1071(4) 0.8202(2) 0.0188(6) Uani 1 1 d .
O4 O 0.6123(3) 0.2443(4) 0.6943(2) 0.0177(6) Uani 1 1 d .
O5 O 0.5822(3) 0.1570(4) 0.8820(2) 0.0229(7) Uani 1 1 d .
O6 O 0.7475(3) 0.3614(4) 0.8439(2) 0.0192(6) Uani 1 1 d .
O7 O 0.5550(2) -0.1356(4) 0.6052(2) 0.0162(6) Uani 1 1 d .
O8 O 0.7420(3) -0.0920(3) 0.5186(2) 0.0151(6) Uani 1 1 d .
O9 O 0.7380(3) -0.3358(3) 0.6296(2) 0.0172(6) Uani 1 1 d .
P1 P 0.95864(9) 0.09506(14) 0.72701(8) 0.01268(19) Uani 1 1 d .
P2 P 0.68623(10) 0.18940(13) 0.80405(8) 0.0140(2) Uani 1 1 d .
P3 P 0.70469(9) -0.14422(13) 0.63356(8) 0.0128(2) Uani 1 1 d .
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'
Br Br -0.2901 2.4595 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C2 C1 Ni1 66.6(2) y
C1 C2 C3 115.9(4) y
C1 C2 Ni1 73.8(3) y
C3 C2 Ni1 73.9(2) y
C2 C3 Ni1 66.5(2) y
C2 Ni1 C1 39.57(18) y
C2 Ni1 C3 39.59(17) y
C1 Ni1 C3 68.42(17) y
C2 Ni1 P1 111.69(14) y
C1 Ni1 P1 151.15(13) y
C3 Ni1 P1 89.03(13) y
C2 Ni1 P2 111.75(14) y
C1 Ni1 P2 93.81(13) y
C3 Ni1 P2 149.80(13) y
P1 Ni1 P2 97.88(4) y
C2 Ni1 P3 123.67(15) y
C1 Ni1 P3 98.33(14) y
C3 Ni1 P3 102.24(13) y
P1 Ni1 P3 104.07(4) y
P2 Ni1 P3 104.46(4) y
C4 O1 P1 120.3(3) y
C5 O2 P1 124.0(3) y
C6 O3 P1 126.5(3) y
C7 O4 P2 122.4(3) y
C8 O5 P2 125.8(3) y
C9 O6 P2 118.2(3) y
C10 O7 P3 121.2(3) y
C11 O8 P3 119.3(3) y
C12 O9 P3 122.1(3) y
O2 P1 O3 108.10(17) y
O2 P1 O1 98.70(15) y
O3 P1 O1 104.60(15) y
O2 P1 Ni1 113.41(11) y
O3 P1 Ni1 110.97(11) y
O1 P1 Ni1 119.85(12) y
O5 P2 O4 105.83(16) y
O5 P2 O6 103.89(16) y
O4 P2 O6 100.44(16) y
O5 P2 Ni1 112.89(12) y
O4 P2 Ni1 109.69(11) y
O6 P2 Ni1 122.39(12) y
O9 P3 O8 98.64(15) y
O9 P3 O7 104.86(16) y
O8 P3 O7 97.15(15) y
O9 P3 Ni1 110.72(12) y
O8 P3 Ni1 120.64(11) y
O7 P3 Ni1 121.48(11) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.387(6) y
C1 Ni1 2.090(4) y
C2 C3 1.388(6) y
C2 Ni1 1.998(4) y
C3 Ni1 2.092(4) y
C4 O1 1.436(5) y
C5 O2 1.442(5) y
C6 O3 1.454(5) y
C7 O4 1.445(5) y
C8 O5 1.452(5) y
C9 O6 1.445(5) y
C10 O7 1.453(5) y
C11 O8 1.439(5) y
C12 O9 1.435(5) y
Ni1 P1 2.1507(11) y
Ni1 P2 2.1805(11) y
Ni1 P3 2.2235(12) y
O1 P1 1.607(3) y
O2 P1 1.586(3) y
O3 P1 1.592(3) y
O4 P2 1.589(3) y
O5 P2 1.587(3) y
O6 P2 1.601(3) y
O7 P3 1.608(3) y
O8 P3 1.608(3) y
O9 P3 1.597(3) y
