#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:49:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178725 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/36/4083688.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_4083688
loop_
_publ_author_name
'Choualeb, Aldjia'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
 Hydridic Rhenium Nitrosyl Complexes with Pincer-Type PNP Ligands
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3509
_journal_paper_doi               10.1021/om070206+
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C16 H39 N2 O P2 Re'
_chemical_formula_sum            'C16 H39 N2 O P2 Re'
_chemical_formula_weight         523.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   14.3447(2)
_cell_length_b                   13.4055(2)
_cell_length_c                   21.8565(4)
_cell_measurement_reflns_used    28160
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     4202.96(12)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.1'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28160
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.939
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.577
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0370
_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)+(0.0432P)²+5.7552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                3689
_reflns_number_total             4816
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om070206%2Bsi20070306_025213.cif
_cod_data_source_block           k0738a
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4083688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.170236(11) 0.383441(13) 0.366664(9) 0.01560(8) Uani 1 1 d .
H1RE H 0.068(3) 0.332(4) 0.395(2) 0.019 Uiso 1 1 d .
H2RE H 0.284(3) 0.380(3) 0.337(2) 0.019 Uiso 1 1 d .
P1 P 0.12017(8) 0.34702(9) 0.26626(6) 0.0183(3) Uani 1 1 d .
P2 P 0.22935(8) 0.36043(9) 0.46786(6) 0.0187(3) Uani 1 1 d .
O1 O 0.1212(3) 0.5995(2) 0.36402(17) 0.0279(9) Uani 1 1 d .
N1 N 0.1999(3) 0.2176(3) 0.36476(19) 0.0215(9) Uani 1 1 d .
H1C H 0.2623 0.2109 0.3539 0.026 Uiso 1 1 calc R
N2 N 0.1423(3) 0.5108(3) 0.36629(19) 0.0207(9) Uani 1 1 d .
C1 C 0.1504(3) 0.2142(4) 0.2564(2) 0.0234(11) Uani 1 1 d .
H1A H 0.1062 0.1824 0.2276 0.028 Uiso 1 1 calc R
H1B H 0.2140 0.2082 0.2393 0.028 Uiso 1 1 calc R
C2 C 0.1457(3) 0.1620(4) 0.3181(2) 0.0243(11) Uani 1 1 d .
H2A H 0.0799 0.1569 0.3314 0.029 Uiso 1 1 calc R
H2B H 0.1710 0.0936 0.3142 0.029 Uiso 1 1 calc R
C3 C 0.1898(3) 0.1701(4) 0.4256(2) 0.0236(11) Uani 1 1 d .
H3A H 0.2089 0.0992 0.4232 0.028 Uiso 1 1 calc R
H3B H 0.1238 0.1726 0.4386 0.028 Uiso 1 1 calc R
C4 C 0.2504(4) 0.2247(3) 0.4720(3) 0.0256(11) Uani 1 1 d .
H4A H 0.3170 0.2107 0.4635 0.031 Uiso 1 1 calc R
H4B H 0.2360 0.2004 0.5137 0.031 Uiso 1 1 calc R
C5 C -0.0043(3) 0.3594(4) 0.2447(2) 0.0258(11) Uani 1 1 d .
H5A H -0.0085 0.3607 0.1990 0.031 Uiso 1 1 calc R
C6 C -0.0632(4) 0.2723(4) 0.2681(4) 0.0445(16) Uani 1 1 d .
H6A H -0.1282 0.2818 0.2555 0.067 Uiso 1 1 calc R
H6B H -0.0597 0.2696 0.3128 0.067 Uiso 1 1 calc R
H6C H -0.0396 0.2097 0.2509 0.067 Uiso 1 1 calc R
C7 C -0.0431(4) 0.4576(4) 0.2693(3) 0.0351(14) Uani 1 1 d .
H7A H -0.1089 0.4638 0.2577 0.053 Uiso 1 1 calc R
H7B H -0.0078 0.5134 0.2520 0.053 Uiso 1 1 calc R
H7C H -0.0377 0.4585 0.3140 0.053 Uiso 1 1 calc R
C8 C 0.1845(3) 0.4061(4) 0.2028(2) 0.0243(11) Uani 1 1 d .
H8A H 0.2516 0.3900 0.2102 0.029 Uiso 1 1 calc R
C9 C 0.1629(4) 0.3662(5) 0.1385(3) 0.0378(16) Uani 1 1 d .
H9A H 0.2010 0.4018 0.1084 0.057 Uiso 1 1 calc R
H9B H 0.0968 0.3764 0.1293 0.057 Uiso 1 1 calc R
H9C H 0.1773 0.2948 0.1368 0.057 Uiso 1 1 calc R
C10 C 0.1784(4) 0.5189(4) 0.2043(3) 0.0377(15) Uani 1 1 d .
H10A H 0.2136 0.5467 0.1698 0.057 Uiso 1 1 calc R
H10B H 0.2047 0.5436 0.2428 0.057 Uiso 1 1 calc R
H10C H 0.1130 0.5394 0.2012 0.057 Uiso 1 1 calc R
C11 C 0.3431(3) 0.4112(4) 0.4946(2) 0.0234(11) Uani 1 1 d .
H11A H 0.3328 0.4826 0.5059 0.028 Uiso 1 1 calc R
C12 C 0.4167(3) 0.4094(4) 0.4439(3) 0.0292(12) Uani 1 1 d .
H12A H 0.4753 0.4369 0.4595 0.044 Uiso 1 1 calc R
H12B H 0.3951 0.4495 0.4092 0.044 Uiso 1 1 calc R
H12C H 0.4267 0.3404 0.4305 0.044 Uiso 1 1 calc R
C13 C 0.3818(4) 0.3578(5) 0.5518(2) 0.0336(13) Uani 1 1 d .
H13A H 0.4413 0.3882 0.5635 0.050 Uiso 1 1 calc R
H13B H 0.3914 0.2870 0.5426 0.050 Uiso 1 1 calc R
H13C H 0.3372 0.3644 0.5855 0.050 Uiso 1 1 calc R
C14 C 0.1524(3) 0.3896(4) 0.5337(2) 0.0211(11) Uani 1 1 d .
H14A H 0.1876 0.3764 0.5724 0.025 Uiso 1 1 calc R
C15 C 0.0641(3) 0.3253(4) 0.5339(3) 0.0291(12) Uani 1 1 d .
H15A H 0.0257 0.3424 0.5694 0.044 Uiso 1 1 calc R
H15B H 0.0815 0.2546 0.5359 0.044 Uiso 1 1 calc R
H15C H 0.0285 0.3376 0.4963 0.044 Uiso 1 1 calc R
C16 C 0.1253(4) 0.5004(4) 0.5323(3) 0.0293(12) Uani 1 1 d .
H16A H 0.0850 0.5155 0.5673 0.044 Uiso 1 1 calc R
H16B H 0.0918 0.5149 0.4942 0.044 Uiso 1 1 calc R
H16C H 0.1817 0.5414 0.5344 0.044 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'
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'
Re Re -1.0185 7.2310 '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
H1RE Re1 H2RE 155(2)
H1RE Re1 N2 101.5(16)
H2RE Re1 N2 103.5(14)
H1RE Re1 N1 76.8(16)
H2RE Re1 N1 78.2(14)
N2 Re1 N1 177.29(17)
H1RE Re1 P1 89.4(16)
H2RE Re1 P1 86.1(17)
N2 Re1 P1 97.33(14)
N1 Re1 P1 80.61(11)
H1RE Re1 P2 85.4(16)
H2RE Re1 P2 90.7(17)
N2 Re1 P2 102.18(14)
N1 Re1 P2 79.83(11)
P1 Re1 P2 160.43(4)
C8 P1 C1 102.1(2)
C8 P1 C5 104.6(2)
C1 P1 C5 106.4(2)
C8 P1 Re1 117.28(17)
C1 P1 Re1 103.67(17)
C5 P1 Re1 120.74(17)
C4 P2 C14 105.5(2)
C4 P2 C11 101.6(2)
C14 P2 C11 101.6(2)
C4 P2 Re1 103.31(18)
C14 P2 Re1 118.66(17)
C11 P2 Re1 123.65(18)
C3 N1 C2 110.5(4)
C3 N1 Re1 112.8(3)
C2 N1 Re1 114.1(3)
O1 N2 Re1 177.7(4)
C2 C1 P1 109.3(4)
N1 C2 C1 110.8(4)
N1 C3 C4 109.6(4)
C3 C4 P2 110.4(3)
C7 C5 C6 109.8(5)
C7 C5 P1 109.8(3)
C6 C5 P1 112.3(4)
C10 C8 C9 110.9(5)
C10 C8 P1 112.5(4)
C9 C8 P1 116.0(4)
C12 C11 C13 109.4(4)
C12 C11 P2 111.8(4)
C13 C11 P2 113.5(4)
C15 C14 C16 109.6(4)
C15 C14 P2 112.0(4)
C16 C14 P2 109.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 H1RE 1.73(5)
Re1 H2RE 1.75(5)
Re1 N2 1.754(4)
Re1 N1 2.264(4)
Re1 P1 2.3601(13)
Re1 P2 2.3889(13)
P1 C8 1.845(5)
P1 C1 1.845(5)
P1 C5 1.854(5)
P2 C4 1.847(5)
P2 C14 1.856(5)
P2 C11 1.862(5)
O1 N2 1.227(5)
N1 C3 1.481(6)
N1 C2 1.483(6)
C1 C2 1.520(7)
C3 C4 1.523(7)
C5 C7 1.527(7)
C5 C6 1.530(7)
C8 C10 1.515(8)
C8 C9 1.535(7)
C11 C12 1.530(7)
C11 C13 1.543(7)
C14 C15 1.533(7)
C14 C16 1.535(7)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C O1 0.93 2.25 3.016(6) 138.9 8_655
