#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:31:10 +0100 (vie 25 de mar de 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004806.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_7004806
loop_
_publ_author_name
'Robertson, Stuart D.'
'Chivers, Tristram'
'Akhtar, Javeed'
'Afzaal, Mohammad'
'O'Brien, Paul'
_publ_section_title
;
 Nickel(ii) complexes of heterodichalcogenido and monochalcogenido
 imidodiphosphinate ligands: AACVD synthesis of nickel ditelluride
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              7004
_journal_page_last               7011
_journal_paper_doi               10.1039/b814065k
_journal_year                    2008
_chemical_formula_moiety         'C24 H56 N2 Ni P4 Se2'
_chemical_formula_sum            'C24 H56 N2 Ni P4 Se2'
_chemical_formula_weight         713.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 104.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9748(2)
_cell_length_b                   19.7569(4)
_cell_length_c                   9.3534(2)
_cell_measurement_reflns_used    20328
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1604.9(2)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phiω 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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25896
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.088
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0259
_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)+(0.0443P)²+0.5052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                3339
_reflns_number_total             3644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814065k.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7004806
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 1.0000 0.01770(9) Uani 1 2 d S . .
Se1 Se 0.60228(2) 0.063793(9) 0.84158(2) 0.02395(8) Uani 1 1 d . . .
P1 P 0.65686(5) 0.15668(2) 0.97651(5) 0.01959(11) Uani 1 1 d . . .
C10 C 0.5181(2) 0.22284(10) 0.8925(2) 0.0276(4) Uani 1 1 d . . .
H10A H 0.5317 0.2321 0.7914 0.033 Uiso 1 1 calc R . .
C11 C 0.3520(3) 0.20026(13) 0.8754(3) 0.0495(7) Uani 1 1 d . . .
H11A H 0.2819 0.2355 0.8239 0.074 Uiso 1 1 calc R . .
H11B H 0.3341 0.1925 0.9732 0.074 Uiso 1 1 calc R . .
H11C H 0.3333 0.1582 0.8179 0.074 Uiso 1 1 calc R . .
C12 C 0.5490(3) 0.28900(11) 0.9806(3) 0.0419(5) Uani 1 1 d . . .
H12A H 0.4667 0.3215 0.9399 0.063 Uiso 1 1 calc R . .
H12B H 0.6480 0.3079 0.9737 0.063 Uiso 1 1 calc R . .
H12C H 0.5522 0.2800 1.0843 0.063 Uiso 1 1 calc R . .
C20 C 0.8420(2) 0.19109(10) 0.9592(2) 0.0270(4) Uani 1 1 d . . .
H20A H 0.8507 0.2382 0.9995 0.032 Uiso 1 1 calc R . .
C21 C 0.9777(2) 0.15123(13) 1.0501(3) 0.0388(5) Uani 1 1 d . . .
H21A H 1.0738 0.1744 1.0484 0.058 Uiso 1 1 calc R . .
H21B H 0.9777 0.1057 1.0083 0.058 Uiso 1 1 calc R . .
H21C H 0.9692 0.1478 1.1522 0.058 Uiso 1 1 calc R . .
C22 C 0.8501(3) 0.19582(13) 0.7986(3) 0.0399(5) Uani 1 1 d . . .
H22A H 0.9474 0.2172 0.7940 0.060 Uiso 1 1 calc R . .
H22B H 0.7637 0.2230 0.7424 0.060 Uiso 1 1 calc R . .
H22C H 0.8444 0.1503 0.7560 0.060 Uiso 1 1 calc R . .
N1 N 0.65991(18) 0.14215(8) 1.14447(17) 0.0224(3) Uani 1 1 d . . .
P2 P 0.61246(5) 0.06601(2) 1.19139(5) 0.01850(11) Uani 1 1 d . . .
C30 C 0.5031(2) 0.08398(10) 1.3303(2) 0.0245(4) Uani 1 1 d . . .
H30A H 0.4913 0.0406 1.3814 0.029 Uiso 1 1 calc R . .
C31 C 0.3425(3) 0.11007(11) 1.2547(3) 0.0341(5) Uani 1 1 d . . .
H31A H 0.2841 0.1174 1.3289 0.051 Uiso 1 1 calc R . .
H31B H 0.2891 0.0767 1.1822 0.051 Uiso 1 1 calc R . .
H31C H 0.3513 0.1529 1.2045 0.051 Uiso 1 1 calc R . .
C32 C 0.5875(3) 0.13423(11) 1.4469(2) 0.0331(5) Uani 1 1 d . . .
H32A H 0.5284 0.1411 1.5206 0.050 Uiso 1 1 calc R . .
H32B H 0.5988 0.1775 1.3994 0.050 Uiso 1 1 calc R . .
H32C H 0.6896 0.1163 1.4954 0.050 Uiso 1 1 calc R . .
C40 C 0.7935(2) 0.02643(9) 1.3025(2) 0.0251(4) Uani 1 1 d . . .
H40A H 0.8628 0.0641 1.3503 0.030 Uiso 1 1 calc R . .
C41 C 0.7741(3) -0.02097(11) 1.4265(2) 0.0351(5) Uani 1 1 d . . .
H41A H 0.8736 -0.0415 1.4743 0.053 Uiso 1 1 calc R . .
H41B H 0.6999 -0.0566 1.3848 0.053 Uiso 1 1 calc R . .
H41C H 0.7364 0.0050 1.4996 0.053 Uiso 1 1 calc R . .
C42 C 0.8756(3) -0.01071(12) 1.2006(3) 0.0364(5) Uani 1 1 d . . .
H42A H 0.9801 -0.0229 1.2562 0.055 Uiso 1 1 calc R . .
H42B H 0.8811 0.0188 1.1179 0.055 Uiso 1 1 calc R . .
H42C H 0.8183 -0.0519 1.1625 0.055 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
P2 Ni1 P2 180.0 3_657 . ?
P2 Ni1 Se1 91.329(19) 3_657 3_657 ?
P2 Ni1 Se1 88.67(2) . 3_657 ?
P2 Ni1 Se1 88.671(19) 3_657 . ?
P2 Ni1 Se1 91.329(19) . . ?
Se1 Ni1 Se1 180.0 3_657 . ?
P1 Se1 Ni1 98.84(2) . . ?
N1 P1 C10 113.04(9) . . ?
N1 P1 C20 111.28(9) . . ?
C10 P1 C20 103.22(9) . . ?
N1 P1 Se1 111.11(6) . . ?
C10 P1 Se1 108.51(7) . . ?
C20 P1 Se1 109.35(7) . . ?
C11 C10 C12 110.2(2) . . ?
C11 C10 P1 112.05(15) . . ?
C12 C10 P1 111.44(16) . . ?
C21 C20 C22 110.66(19) . . ?
C21 C20 P1 111.93(15) . . ?
C22 C20 P1 112.21(14) . . ?
P1 N1 P2 119.02(10) . . ?
N1 P2 C30 103.29(9) . . ?
N1 P2 C40 106.44(9) . . ?
C30 P2 C40 103.35(9) . . ?
N1 P2 Ni1 114.35(6) . . ?
C30 P2 Ni1 117.48(7) . . ?
C40 P2 Ni1 110.79(7) . . ?
C31 C30 C32 110.59(18) . . ?
C31 C30 P2 110.22(14) . . ?
C32 C30 P2 111.75(14) . . ?
C42 C40 C41 110.03(17) . . ?
C42 C40 P2 110.02(14) . . ?
C41 C40 P2 115.33(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P2 2.2388(7) 3_657 ?
Ni1 P2 2.2388(7) . ?
Ni1 Se1 2.3051(5) 3_657 ?
Ni1 Se1 2.3051(4) . ?
Se1 P1 2.2109(6) . ?
P1 N1 1.5905(17) . ?
P1 C10 1.839(2) . ?
P1 C20 1.8402(19) . ?
C10 C11 1.526(3) . ?
C10 C12 1.533(3) . ?
C20 C21 1.518(3) . ?
C20 C22 1.525(3) . ?
N1 P2 1.6527(16) . ?
P2 C30 1.850(2) . ?
P2 C40 1.866(2) . ?
C30 C31 1.526(3) . ?
C30 C32 1.527(3) . ?
C40 C42 1.531(3) . ?
C40 C41 1.534(3) . ?
