#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/11/4321178.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_4321178
loop_
_publ_author_name
'Gabriele Albertin'
'Stefano Antoniutti'
'Alessia Bacchi'
'Emilio Bordignon'
'Francesca Miani'
'Giancarlo Pelizzi'
_publ_section_title
;
 Diazo Complexes of Rhenium: Preparations and Crystal Structures of the
 Bis(dinitrogen), [Re(N2)2{PPh(OEt)2}4][BPh4] and Methyldiazenido
 [ReCl(CH3N2)(CH3NHNH2){PPh(OEt)2}3][BPh4] Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3283
_journal_page_last               3293
_journal_paper_doi               10.1021/ic990970r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C64 H80 B N4 O8 P4 Re'
_chemical_formula_weight         1354.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2b'
_symmetry_space_group_name_H-M   'P b a 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                   23.008(5)
_cell_length_b                   23.367(5)
_cell_length_c                   12.863(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.41
_cell_measurement_theta_min      4.78
_cell_volume                     6916(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .918
_diffrn_measured_fraction_theta_max .918
_diffrn_measurement_device_type  'Philips PW100 diffractometer'
_diffrn_measurement_method       'θ/2θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19904
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        25
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .442
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2784
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.652
_refine_diff_density_rms         .098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         10103
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0513P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3846
_reflns_number_total             10103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990970r_1.cif
_cod_data_source_block           Compound_[Re(N2)2{PPh(OEt)2}4]BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'othorhombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C64 H80 B1 N4 O8 P4 Re1'
_cod_database_code               4321178
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z'
'x-1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.2500 0.0000 0.11833(2) 0.04342(10) Uani 1 d SD . .
P1 P 0.35193(7) 0.02897(7) 0.12910(14) 0.0558(4) Uani 1 d . . .
P2 P 0.22042(7) 0.09992(6) 0.12565(13) 0.0522(4) Uani 1 d . . .
O1 O 0.35890(18) 0.09727(16) 0.1256(4) 0.0767(14) Uani 1 d . . .
O2 O 0.39758(19) 0.00595(19) 0.0457(4) 0.0737(12) Uani 1 d . . .
O3 O 0.15251(17) 0.10693(15) 0.0993(3) 0.0624(12) Uani 1 d . . .
O4 O 0.2508(2) 0.14684(15) 0.0530(3) 0.0676(11) Uani 1 d . . .
C199 C 0.2500 0.0000 0.639(2) 0.147(14) Uani 0.50 d SP . .
C200 C 0.1937(9) 0.0137(11) 0.6471(17) 0.127(8) Uani 0.50 d P . .
C201 C 0.2321(11) 0.0554(8) 0.6584(16) 0.137(9) Uani 0.50 d P . .
N1 N 0.2500 0.0000 0.2758(5) 0.0530(16) Uani 0.911(4) d SPDU A 1
N2 N 0.2500 0.0000 0.3553(5) 0.0565(16) Uani 0.911(4) d SPDU A 1
Cl Cl 0.2500 0.0000 0.3078(12) 0.0529(17) Uani 0.089(4) d SPDU A 2
N3 N 0.2500 0.0000 -0.0348(7) 0.070(2) Uani 1 d SU . .
N4 N 0.2500 0.0000 -0.1198(9) 0.155(6) Uani 1 d SU . .
B B 0.5012(6) 0.2500 0.5000 0.063(3) Uani 0.911(4) d SP . 1
C1 C 0.3911(3) 0.0082(3) 0.2449(5) 0.0613(17) Uani 1 d . . .
C2 C 0.3793(3) 0.0371(3) 0.3363(6) 0.082(2) Uani 1 d . . .
H2 H 0.3531 0.0674 0.3378 0.098 Uiso 1 calc R . .
C3 C 0.4087(5) 0.0187(4) 0.4287(7) 0.118(3) Uani 1 d . . .
H3 H 0.4026 0.0379 0.4911 0.141 Uiso 1 calc R . .
C4 C 0.4465(4) -0.0279(4) 0.4248(9) 0.123(4) Uani 1 d . . .
H4 H 0.4641 -0.0408 0.4856 0.147 Uiso 1 calc R . .
C5 C 0.4577(4) -0.0540(4) 0.3354(8) 0.103(3) Uani 1 d . . .
H5 H 0.4833 -0.0848 0.3339 0.123 Uiso 1 calc R . .
C6 C 0.4317(3) -0.0359(3) 0.2449(7) 0.079(2) Uani 1 d . . .
H6 H 0.4414 -0.0535 0.1824 0.094 Uiso 1 calc R . .
C7 C 0.4157(3) 0.1240(3) 0.1411(9) 0.149(5) Uani 1 d . . .
H7A H 0.4231 0.1277 0.2150 0.179 Uiso 1 calc R . .
H7B H 0.4456 0.0995 0.1119 0.179 Uiso 1 calc R . .
C8 C 0.4191(4) 0.1767(3) 0.0958(9) 0.172(6) Uani 1 d . . .
H8A H 0.4277 0.1724 0.0232 0.207 Uiso 1 calc R . .
H8B H 0.4494 0.1985 0.1285 0.207 Uiso 1 calc R . .
H8C H 0.3827 0.1962 0.1038 0.207 Uiso 1 calc R . .
C9 C 0.3870(4) 0.0074(5) -0.0624(7) 0.152(5) Uani 1 d . . .
H9A H 0.3603 -0.0233 -0.0796 0.182 Uiso 1 calc R . .
H9B H 0.3680 0.0432 -0.0791 0.182 Uiso 1 calc R . .
C10 C 0.4353(5) 0.0021(4) -0.1235(7) 0.173(6) Uani 1 d . . .
H10A H 0.4611 0.0335 -0.1105 0.208 Uiso 1 calc R . .
H10B H 0.4240 0.0022 -0.1953 0.208 Uiso 1 calc R . .
H10C H 0.4547 -0.0332 -0.1076 0.208 Uiso 1 calc R . .
C11 C 0.2294(3) 0.1350(2) 0.2495(5) 0.0588(18) Uani 1 d . . .
C12 C 0.2734(3) 0.1745(3) 0.2692(6) 0.080(2) Uani 1 d . . .
H12 H 0.2990 0.1848 0.2165 0.096 Uiso 1 calc R . .
C13 C 0.2792(4) 0.1985(3) 0.3671(8) 0.106(3) Uani 1 d . . .
H13 H 0.3086 0.2250 0.3800 0.127 Uiso 1 calc R . .
C14 C 0.2416(5) 0.1833(3) 0.4451(7) 0.119(4) Uani 1 d . . .
H14 H 0.2464 0.1988 0.5112 0.143 Uiso 1 calc R . .
C15 C 0.1961(4) 0.1449(3) 0.4268(7) 0.101(3) Uani 1 d . . .
H15 H 0.1698 0.1357 0.4790 0.121 Uiso 1 calc R . .
C16 C 0.1914(3) 0.1208(3) 0.3276(6) 0.076(2) Uani 1 d . . .
H16 H 0.1619 0.0947 0.3143 0.091 Uiso 1 calc R . .
C17 C 0.1236(3) 0.1622(3) 0.1064(7) 0.099(3) Uani 1 d . . .
H17A H 0.1116 0.1690 0.1777 0.119 Uiso 1 calc R . .
H17B H 0.1505 0.1922 0.0867 0.119 Uiso 1 calc R . .
C18 C 0.0743(4) 0.1638(3) 0.0404(8) 0.146(4) Uani 1 d . . .
H18A H 0.0846 0.1489 -0.0268 0.175 Uiso 1 calc R . .
H18B H 0.0612 0.2026 0.0333 0.175 Uiso 1 calc R . .
H18C H 0.0439 0.1409 0.0698 0.175 Uiso 1 calc R . .
C19 C 0.2575(4) 0.1385(3) -0.0566(6) 0.101(3) Uani 1 d . . .
H19A H 0.2239 0.1183 -0.0836 0.122 Uiso 1 calc R . .
H19B H 0.2916 0.1152 -0.0695 0.122 Uiso 1 calc R . .
C20 C 0.2635(4) 0.1922(4) -0.1095(6) 0.132(4) Uani 1 d . . .
H20A H 0.2293 0.2149 -0.0981 0.159 Uiso 1 calc R . .
H20B H 0.2682 0.1854 -0.1826 0.159 Uiso 1 calc R . .
H20C H 0.2969 0.2121 -0.0832 0.159 Uiso 1 calc R . .
C100 C 0.5413(4) 0.2098(3) 0.4263(6) 0.066(2) Uani 0.911(4) d P . 1
C101 C 0.5270(4) 0.1529(4) 0.3995(6) 0.085(3) Uani 0.911(4) d P . 1
H101 H 0.4944 0.1361 0.4294 0.102 Uiso 0.911(4) calc PR A 1
C102 C 0.5601(5) 0.1212(4) 0.3299(7) 0.111(4) Uani 0.911(4) d P . 1
H102 H 0.5491 0.0842 0.3122 0.133 Uiso 0.911(4) calc PR A 1
C103 C 0.6099(6) 0.1454(5) 0.2870(8) 0.129(5) Uani 0.911(4) d P . 1
H103 H 0.6327 0.1240 0.2417 0.155 Uiso 0.911(4) calc PR A 1
C104 C 0.6256(4) 0.2007(5) 0.3108(7) 0.110(4) Uani 0.911(4) d P . 1
H104 H 0.6587 0.2169 0.2815 0.132 Uiso 0.911(4) calc PR A 1
C105 C 0.5917(4) 0.2317(4) 0.3790(7) 0.093(3) Uani 0.911(4) d P . 1
H105 H 0.6027 0.2691 0.3945 0.112 Uiso 0.911(4) calc PR A 1
C106 C 0.4583(4) 0.2112(3) 0.5783(7) 0.070(2) Uani 0.911(4) d P . 1
C107 C 0.4664(4) 0.2052(3) 0.6832(7) 0.093(3) Uani 0.911(4) d P . 1
H107 H 0.4974 0.2243 0.7140 0.111 Uiso 0.911(4) calc PR A 1
C108 C 0.4304(5) 0.1717(4) 0.7464(9) 0.116(4) Uani 0.911(4) d P . 1
H108 H 0.4382 0.1691 0.8172 0.139 Uiso 0.911(4) calc PR A 1
C109 C 0.3867(6) 0.1444(5) 0.7084(10) 0.115(4) Uani 0.911(4) d P . 1
H109 H 0.3639 0.1215 0.7513 0.138 Uiso 0.911(4) calc PR A 1
C110 C 0.3739(4) 0.1490(4) 0.6061(10) 0.111(4) Uani 0.911(4) d P . 1
H110 H 0.3418 0.1298 0.5792 0.133 Uiso 0.911(4) calc PR A 1
C111 C 0.4091(4) 0.1827(3) 0.5396(8) 0.092(3) Uani 0.911(4) d P . 1
H111 H 0.3995 0.1859 0.4696 0.111 Uiso 0.911(4) calc PR A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 '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
N3 Re N1 180.0 . . ?
N3 Re P2 92.22(4) . . ?
N1 Re P2 87.78(4) . . ?
N3 Re P2 92.22(4) . 2 ?
N1 Re P2 87.78(4) . 2 ?
P2 Re P2 175.56(8) . 2 ?
N3 Re Cl 180.0 . . ?
N1 Re Cl 0.0 . . ?
P2 Re Cl 87.78(4) . . ?
P2 Re Cl 87.78(4) 2 . ?
N3 Re P1 93.25(4) . 2 ?
N1 Re P1 86.75(4) . 2 ?
P2 Re P1 89.72(5) . 2 ?
P2 Re P1 90.02(5) 2 2 ?
Cl Re P1 86.75(4) . 2 ?
N3 Re P1 93.25(4) . . ?
N1 Re P1 86.75(4) . . ?
P2 Re P1 90.03(5) . . ?
P2 Re P1 89.72(5) 2 . ?
Cl Re P1 86.75(4) . . ?
P1 Re P1 173.50(9) 2 . ?
O2 P1 O1 104.5(2) . . ?
O2 P1 C1 97.8(3) . . ?
O1 P1 C1 103.9(3) . . ?
O2 P1 Re 120.01(19) . . ?
O1 P1 Re 111.70(17) . . ?
C1 P1 Re 116.8(2) . . ?
O4 P2 O3 103.4(2) . . ?
O4 P2 C11 98.9(3) . . ?
O3 P2 C11 104.5(3) . . ?
O4 P2 Re 120.83(17) . . ?
O3 P2 Re 111.19(15) . . ?
C11 P2 Re 115.98(19) . . ?
C7 O1 P1 120.7(4) . . ?
C9 O2 P1 122.8(5) . . ?
C17 O3 P2 121.4(4) . . ?
C19 O4 P2 122.0(4) . . ?
C200 C199 C200 171(3) . 2 ?
C200 C199 C201 58.2(10) . . ?
C200 C199 C201 120.1(12) 2 . ?
C200 C199 C201 120.1(12) . 2 ?
C200 C199 C201 58.2(10) 2 2 ?
C201 C199 C201 160(3) . 2 ?
C201 C200 C199 62.5(13) . . ?
C200 C201 C199 59.3(13) . . ?
N2 N1 Re 180.0 . . ?
N4 N3 Re 180.0 . . ?
C100 B C100 110.8(11) . 3_556 ?
C100 B C106 111.9(3) . . ?
C100 B C106 107.2(4) 3_556 . ?
C100 B C106 107.2(4) . 3_556 ?
C100 B C106 111.9(3) 3_556 3_556 ?
C106 B C106 107.9(10) . 3_556 ?
C2 C1 C6 119.6(7) . . ?
C2 C1 P1 118.2(6) . . ?
C6 C1 P1 122.2(6) . . ?
C1 C2 C3 117.7(8) . . ?
C4 C3 C2 120.0(9) . . ?
C5 C4 C3 120.7(10) . . ?
C4 C5 C6 120.6(10) . . ?
C5 C6 C1 121.3(8) . . ?
C8 C7 O1 112.3(7) . . ?
C10 C9 O2 115.1(10) . . ?
C16 C11 C12 119.3(6) . . ?
C16 C11 P2 117.7(5) . . ?
C12 C11 P2 123.0(6) . . ?
C13 C12 C11 120.2(8) . . ?
C14 C13 C12 119.9(8) . . ?
C13 C14 C15 121.0(8) . . ?
C14 C15 C16 118.0(8) . . ?
C11 C16 C15 121.5(7) . . ?
C18 C17 O3 110.5(7) . . ?
O4 C19 C20 111.1(6) . . ?
C105 C100 C101 115.5(7) . . ?
C105 C100 B 120.6(8) . . ?
C101 C100 B 123.8(8) . . ?
C102 C101 C100 122.1(8) . . ?
C101 C102 C103 119.4(9) . . ?
C104 C103 C102 120.6(10) . . ?
C103 C104 C105 119.1(10) . . ?
C104 C105 C100 123.3(9) . . ?
C107 C106 C111 114.3(9) . . ?
C107 C106 B 124.5(8) . . ?
C111 C106 B 121.2(8) . . ?
C106 C107 C108 123.2(10) . . ?
C109 C108 C107 121.3(12) . . ?
C108 C109 C110 119.9(13) . . ?
C109 C110 C111 120.6(11) . . ?
C106 C111 C110 120.6(10) . . ?
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
Re N3 1.970(9) . ?
Re N1 2.025(7) . ?
Re P2 2.4339(15) . ?
Re P2 2.4340(15) 2 ?
Re Cl 2.437(16) . ?
Re P1 2.4448(16) 2 ?
Re P1 2.4449(16) . ?
P1 O2 1.595(4) . ?
P1 O1 1.605(4) . ?
P1 C1 1.807(7) . ?
P2 O4 1.601(4) . ?
P2 O3 1.607(4) . ?
P2 C11 1.803(6) . ?
O1 C7 1.462(8) . ?
O2 C9 1.411(10) . ?
O3 C17 1.455(7) . ?
O4 C19 1.432(8) . ?
C199 C200 1.34(2) . ?
C199 C200 1.34(2) 2 ?
C199 C201 1.38(2) . ?
C199 C201 1.38(2) 2 ?
C200 C201 1.32(2) . ?
N1 N2 1.022(2) . ?
N3 N4 1.092(12) . ?
B C100 1.623(10) . ?
B C100 1.623(10) 3_556 ?
B C106 1.677(10) . ?
B C106 1.677(10) 3_556 ?
C1 C2 1.383(9) . ?
C1 C6 1.391(9) . ?
C2 C3 1.433(11) . ?
C3 C4 1.395(13) . ?
C4 C5 1.327(12) . ?
C5 C6 1.375(10) . ?
C7 C8 1.363(10) . ?
C9 C10 1.366(12) . ?
C11 C16 1.372(8) . ?
C11 C12 1.396(9) . ?
C12 C13 1.385(10) . ?
C13 C14 1.372(12) . ?
C14 C15 1.397(10) . ?
C15 C16 1.398(9) . ?
C17 C18 1.418(10) . ?
C19 C20 1.432(10) . ?
C100 C105 1.406(11) . ?
C100 C101 1.412(10) . ?
C101 C102 1.389(10) . ?
C102 C103 1.390(14) . ?
C103 C104 1.377(13) . ?
C104 C105 1.381(11) . ?
C106 C107 1.369(11) . ?
C106 C111 1.406(11) . ?
C107 C108 1.400(11) . ?
C108 C109 1.288(14) . ?
C109 C110 1.353(13) . ?
C110 C111 1.416(11) . ?
