#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:55:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179161 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312264.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_4312264
loop_
_publ_author_name
'Francesco Tisato'
'Fiorenzo Refosco'
'Marina Porchia'
'Cristina Bolzati'
'Giuliano Bandoli'
'Alessandro Dolmella'
'Adriano Duatti'
'Alessandra Boschi'
'Christian M. Jung'
'Hans-Juergen Pietzsch'
'Werner Kraus'
_publ_section_title
;
 The Crucial Role of the Diphosphine Heteroatom X in the Stereochemistry
 and Stabilization of the Substitution-Inert [M(N)(PXP)]2+ Metal Fragments
 (M = Tc, Re; PXP = Diphosphine Ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8617
_journal_page_last               8625
_journal_paper_doi               10.1021/ic049139r
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C29 H31 Cl4 N2 P2 Tc'
_chemical_formula_weight         709.30
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.65(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.310(2)
_cell_length_b                   17.708(3)
_cell_length_c                   15.197(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      7.5
_cell_volume                     3119.8(9)
_computing_cell_refinement       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_computing_publication_material  'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL/NT vers.5.10 (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nicolet R3m/V diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5485
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00000(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          1.741
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                3753
_reflns_number_total             5485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049139rsi20040701_071623.cif
_cod_data_source_block           1.CH2Cl2
_cod_original_cell_volume        3119.8(8)
_cod_database_code               4312264
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
Tc Tc 0.14195(2) 0.133456(16) 0.91190(2) 0.03412(10) Uani 1 1 d . . .
Cl1 Cl 0.34948(8) 0.13604(6) 0.95119(7) 0.0585(3) Uani 1 1 d . . .
Cl2 Cl 0.16272(7) 0.01546(5) 1.02379(7) 0.0477(2) Uani 1 1 d . . .
P1 P 0.09445(8) 0.04675(5) 0.78096(6) 0.0417(2) Uani 1 1 d . . .
P2 P 0.13659(8) 0.20438(5) 1.04722(6) 0.0382(2) Uani 1 1 d . . .
N1 N 0.1059(3) 0.20379(16) 0.8403(2) 0.0469(8) Uani 1 1 d . . .
N2 N -0.0363(2) 0.11186(15) 0.89822(18) 0.0360(7) Uani 1 1 d . . .
C1 C -0.0592(3) 0.0304(2) 0.7628(3) 0.0541(11) Uani 1 1 d . . .
H1A H -0.1009 0.0244 0.6966 0.065 Uiso 1 1 calc R . .
H1B H -0.0675 -0.0159 0.7940 0.065 Uiso 1 1 calc R . .
C2 C -0.1106(3) 0.0950(2) 0.8002(2) 0.0482(10) Uani 1 1 d . . .
H2A H -0.1161 0.1394 0.7615 0.058 Uiso 1 1 calc R . .
H2B H -0.1877 0.0818 0.7986 0.058 Uiso 1 1 calc R . .
C3 C -0.0877(3) 0.1726(2) 0.9392(3) 0.0468(10) Uani 1 1 d . . .
H3A H -0.1649 0.1582 0.9363 0.056 Uiso 1 1 calc R . .
H3B H -0.0931 0.2189 0.9039 0.056 Uiso 1 1 calc R . .
C4 C -0.0125(3) 0.1856(2) 1.0408(3) 0.0486(10) Uani 1 1 d . . .
H4A H -0.0147 0.1413 1.0778 0.058 Uiso 1 1 calc R . .
H4B H -0.0419 0.2282 1.0661 0.058 Uiso 1 1 calc R . .
C5 C 0.1590(3) -0.04509(19) 0.7829(2) 0.0441(9) Uani 1 1 d . . .
C6 C 0.2650(4) -0.0602(2) 0.8485(3) 0.0596(11) Uani 1 1 d . . .
H6A H 0.3014 -0.0237 0.8924 0.071 Uiso 1 1 calc R . .
C7 C 0.3179(4) -0.1295(3) 0.8496(3) 0.0785(14) Uani 1 1 d . . .
H7A H 0.3897 -0.1394 0.8939 0.094 Uiso 1 1 calc R . .
C8 C 0.2634(5) -0.1831(3) 0.7849(4) 0.0781(15) Uani 1 1 d . . .
H8A H 0.2987 -0.2297 0.7854 0.094 Uiso 1 1 calc R . .
C9 C 0.1583(5) -0.1693(3) 0.7200(3) 0.0761(15) Uani 1 1 d . . .
H9A H 0.1220 -0.2064 0.6767 0.091 Uiso 1 1 calc R . .
C10 C 0.1050(4) -0.0997(2) 0.7182(3) 0.0653(12) Uani 1 1 d . . .
H10A H 0.0334 -0.0901 0.6735 0.078 Uiso 1 1 calc R . .
C11 C 0.1024(4) 0.0919(2) 0.6766(2) 0.0490(10) Uani 1 1 d . . .
C12 C 0.2069(4) 0.0931(2) 0.6626(3) 0.0694(13) Uani 1 1 d . . .
H12A H 0.2688 0.0660 0.7023 0.083 Uiso 1 1 calc R . .
C13 C 0.2208(5) 0.1344(3) 0.5899(4) 0.0929(17) Uani 1 1 d . . .
H13A H 0.2919 0.1344 0.5809 0.111 Uiso 1 1 calc R . .
C14 C 0.1323(7) 0.1749(3) 0.5316(4) 0.0957(19) Uani 1 1 d . . .
H14A H 0.1418 0.2016 0.4819 0.115 Uiso 1 1 calc R . .
C15 C 0.0305(6) 0.1761(3) 0.5463(3) 0.0974(19) Uani 1 1 d . . .
H15A H -0.0297 0.2053 0.5082 0.117 Uiso 1 1 calc R . .
C16 C 0.0147(4) 0.1342(3) 0.6176(3) 0.0772(14) Uani 1 1 d . . .
H16A H -0.0569 0.1348 0.6258 0.093 Uiso 1 1 calc R . .
C17 C 0.1501(3) 0.30660(19) 1.0391(2) 0.0406(9) Uani 1 1 d . . .
C18 C 0.1137(4) 0.3556(2) 1.0937(3) 0.0585(11) Uani 1 1 d . . .
H18A H 0.0821 0.3366 1.1369 0.070 Uiso 1 1 calc R . .
C19 C 0.1236(4) 0.4327(2) 1.0850(3) 0.0715(14) Uani 1 1 d . . .
H19A H 0.0983 0.4656 1.1217 0.086 Uiso 1 1 calc R . .
C20 C 0.1707(4) 0.4603(2) 1.0225(3) 0.0744(14) Uani 1 1 d . . .
H20A H 0.1760 0.5122 1.0161 0.089 Uiso 1 1 calc R . .
C21 C 0.2100(4) 0.4134(2) 0.9692(3) 0.0665(13) Uani 1 1 d . . .
H21A H 0.2436 0.4329 0.9276 0.080 Uiso 1 1 calc R . .
C22 C 0.1995(3) 0.3361(2) 0.9775(3) 0.0537(10) Uani 1 1 d . . .
H22A H 0.2261 0.3037 0.9411 0.064 Uiso 1 1 calc R . .
C23 C 0.2263(3) 0.18126(19) 1.1657(2) 0.0421(9) Uani 1 1 d . . .
C24 C 0.1826(4) 0.1669(2) 1.2361(3) 0.0587(11) Uani 1 1 d . . .
H24A H 0.1040 0.1719 1.2255 0.070 Uiso 1 1 calc R . .
C25 C 0.2568(5) 0.1448(2) 1.3235(3) 0.0686(13) Uani 1 1 d . . .
H25A H 0.2272 0.1340 1.3709 0.082 Uiso 1 1 calc R . .
C26 C 0.3724(4) 0.1388(2) 1.3406(3) 0.0667(13) Uani 1 1 d . . .
H26A H 0.4212 0.1238 1.3992 0.080 Uiso 1 1 calc R . .
C27 C 0.4158(4) 0.1546(2) 1.2724(3) 0.0649(12) Uani 1 1 d . . .
H27A H 0.4949 0.1517 1.2845 0.078 Uiso 1 1 calc R . .
C28 C 0.3434(4) 0.1750(2) 1.1845(3) 0.0561(11) Uani 1 1 d . . .
H28A H 0.3742 0.1847 1.1375 0.067 Uiso 1 1 calc R . .
Cl3 Cl 0.58590(13) 0.16800(10) 0.83975(12) 0.1151(5) Uani 1 1 d . . .
Cl4 Cl 0.51128(18) 0.01948(11) 0.77520(15) 0.1528(8) Uani 1 1 d . . .
C29 C 0.5646(4) 0.0764(3) 0.8714(4) 0.1011(19) Uani 1 1 d . . .
H29A H 0.6373 0.0560 0.9121 0.121 Uiso 1 1 calc R . .
H29B H 0.5110 0.0770 0.9058 0.121 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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
N1 Tc N2 91.80(13) . . ?
N1 Tc Cl1 100.36(11) . . ?
N2 Tc Cl1 167.82(8) . . ?
N1 Tc P1 90.00(11) . . ?
N2 Tc P1 81.52(8) . . ?
Cl1 Tc P1 99.08(4) . . ?
N1 Tc P2 95.27(11) . . ?
N2 Tc P2 81.81(7) . . ?
Cl1 Tc P2 96.21(3) . . ?
P1 Tc P2 162.66(4) . . ?
N1 Tc Cl2 170.19(11) . . ?
N2 Tc Cl2 78.39(7) . . ?
Cl1 Tc Cl2 89.46(3) . . ?
P1 Tc Cl2 88.39(3) . . ?
P2 Tc Cl2 83.61(3) . . ?
C11 P1 C5 105.01(17) . . ?
C11 P1 C1 107.09(19) . . ?
C5 P1 C1 106.56(18) . . ?
C11 P1 Tc 111.78(12) . . ?
C5 P1 Tc 125.01(12) . . ?
C1 P1 Tc 100.07(13) . . ?
C23 P2 C17 104.60(16) . . ?
C23 P2 C4 106.02(17) . . ?
C17 P2 C4 106.75(17) . . ?
C23 P2 Tc 122.86(12) . . ?
C17 P2 Tc 115.23(12) . . ?
C4 P2 Tc 99.95(12) . . ?
C3 N2 C2 111.0(3) . . ?
C3 N2 Tc 113.1(2) . . ?
C2 N2 Tc 113.0(2) . . ?
C2 C1 P1 111.3(2) . . ?
N2 C2 C1 109.5(3) . . ?
N2 C3 C4 109.5(3) . . ?
C3 C4 P2 109.6(2) . . ?
C6 C5 C10 119.5(4) . . ?
C6 C5 P1 119.5(3) . . ?
C10 C5 P1 121.0(3) . . ?
C5 C6 C7 120.6(4) . . ?
C8 C7 C6 119.3(4) . . ?
C9 C8 C7 120.8(4) . . ?
C8 C9 C10 120.1(4) . . ?
C5 C10 C9 119.7(4) . . ?
C12 C11 C16 117.5(4) . . ?
C12 C11 P1 118.2(3) . . ?
C16 C11 P1 123.6(3) . . ?
C11 C12 C13 120.4(5) . . ?
C14 C13 C12 120.9(5) . . ?
C15 C14 C13 119.2(5) . . ?
C14 C15 C16 120.6(5) . . ?
C11 C16 C15 121.3(5) . . ?
C18 C17 C22 118.6(4) . . ?
C18 C17 P2 121.9(3) . . ?
C22 C17 P2 119.5(3) . . ?
C17 C18 C19 120.5(4) . . ?
C20 C19 C18 119.6(4) . . ?
C21 C20 C19 121.3(4) . . ?
C20 C21 C22 119.1(4) . . ?
C17 C22 C21 120.9(4) . . ?
C24 C23 C28 118.7(4) . . ?
C24 C23 P2 123.2(3) . . ?
C28 C23 P2 118.0(3) . . ?
C23 C24 C25 119.5(4) . . ?
C26 C25 C24 120.8(4) . . ?
C27 C26 C25 119.8(4) . . ?
C26 C27 C28 120.3(4) . . ?
C23 C28 C27 120.8(4) . . ?
Cl4 C29 Cl3 111.3(3) . . ?
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
Tc N1 1.614(3) . ?
Tc N2 2.167(3) . ?
Tc Cl1 2.4206(10) . ?
Tc P1 2.4241(10) . ?
Tc P2 2.4294(10) . ?
Tc Cl2 2.6515(10) . ?
P1 C11 1.807(4) . ?
P1 C5 1.806(4) . ?
P1 C1 1.840(4) . ?
P2 C23 1.814(4) . ?
P2 C17 1.826(4) . ?
P2 C4 1.835(4) . ?
N2 C3 1.486(4) . ?
N2 C2 1.493(4) . ?
C1 C2 1.508(5) . ?
C3 C4 1.527(5) . ?
C5 C6 1.376(5) . ?
C5 C10 1.380(5) . ?
C6 C7 1.386(5) . ?
C7 C8 1.370(6) . ?
C8 C9 1.360(6) . ?
C9 C10 1.392(6) . ?
C11 C12 1.374(5) . ?
C11 C16 1.372(5) . ?
C12 C13 1.383(6) . ?
C13 C14 1.357(7) . ?
C14 C15 1.345(7) . ?
C15 C16 1.379(6) . ?
C17 C18 1.376(5) . ?
C17 C22 1.379(5) . ?
C18 C19 1.382(5) . ?
C19 C20 1.358(6) . ?
C20 C21 1.358(6) . ?
C21 C22 1.383(5) . ?
C23 C24 1.374(5) . ?
C23 C28 1.376(5) . ?
C24 C25 1.391(5) . ?
C25 C26 1.362(6) . ?
C26 C27 1.345(6) . ?
C27 C28 1.382(5) . ?
Cl3 C29 1.737(6) . ?
Cl4 C29 1.714(6) . ?
