#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:40:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179983 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/77/7027760.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027760
loop_
_publ_author_name
'Wagner, Gabriele'
'Pombeiro, Armando J. L.'
'Bokach, Nadezhda A.'
'Kukushkin, Vadim Yu.'
_publ_section_title
;
 Facile rhenium(IV)-mediated coupling of acetonitrile and
 oximes †
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4083
_journal_paper_doi               10.1039/a906455i
_journal_year                    1999
_chemical_formula_sum            'C24 H44 Cl4 N4 O2 Re'
_chemical_formula_weight         748.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.890(2)
_cell_length_b                   16.460(3)
_cell_length_c                   19.921(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     3242.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.518
_diffrn_measured_fraction_theta_max 0.518
_diffrn_measurement_device_type  CAD-4
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  beta-filter
_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    0.0226
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1662
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.102
_exptl_absorpt_correction_T_max  0.6388
_exptl_absorpt_correction_T_min  0.2841
_exptl_absorpt_correction_type   numeric
_exptl_crystal_colour            blueish(?)
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.038(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0702P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                1662
_reflns_number_total             1662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906455Isup1.cif
_cod_data_source_block           vk16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0702P)^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^)+(0.0702P)^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_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7027760
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'
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
Re Re 0.47327(5) 0.50288(5) 0.467126(18) 0.05231(18) Uani 1 d
Cl1 Cl 0.3736(4) 0.6089(3) 0.5277(2) 0.0802(12) Uani 1 d
Cl2 Cl 0.4727(5) 0.5781(3) 0.36883(17) 0.0892(14) Uani 1 d
Cl3 Cl 0.5946(6) 0.3991(2) 0.4168(2) 0.0944(15) Uani 1 d
Cl4 Cl 0.2653(5) 0.4439(3) 0.4446(2) 0.1066(18) Uani 1 d
O1 O 0.4559(12) 0.3520(5) 0.6479(4) 0.066(3) Uani 1 d
O2 O 0.8472(9) 0.6224(5) 0.5274(4) 0.054(2) Uani 1 d
N1 N 0.4773(12) 0.4437(7) 0.5617(4) 0.060(3) Uani 1 d
N2 N 0.4839(12) 0.4220(6) 0.6914(4) 0.049(3) Uani 1 d
N3 N 0.6637(10) 0.5474(7) 0.4973(5) 0.048(2) Uani 1 d
N4 N 0.8985(12) 0.5443(6) 0.5524(5) 0.052(3) Uani 1 d
C1 C 0.4373(13) 0.4089(8) 0.7505(6) 0.053(4) Uani 1 d
C2 C 0.4609(16) 0.4716(9) 0.8041(6) 0.060(4) Uani 1 d
C3 C 0.529(2) 0.4260(10) 0.8648(7) 0.078(5) Uani 1 d
C4 C 0.449(2) 0.3543(9) 0.8869(6) 0.082(5) Uani 1 d
C5 C 0.4238(16) 0.2940(9) 0.8312(6) 0.072(4) Uani 1 d
C6 C 0.3549(16) 0.3361(9) 0.7722(6) 0.062(4) Uani 1 d
C7 C 0.5406(18) 0.5461(10) 0.7800(7) 0.069(4) Uani 1 d
C8 C 0.523(3) 0.6153(10) 0.8297(9) 0.106(7) Uani 1 d
C9 C 0.6913(16) 0.5309(10) 0.7668(8) 0.078(5) Uani 1 d
C10 C 0.340(2) 0.2203(11) 0.8536(7) 0.102(7) Uani 1 d
C11 C 0.4629(17) 0.3718(8) 0.5822(6) 0.059(3) Uani 1 d
C12 C 0.4447(17) 0.2968(8) 0.5413(6) 0.069(4) Uani 1 d
C13 C 0.9921(15) 0.5532(8) 0.5954(7) 0.047(4) Uani 1 d
C14 C 1.0564(14) 0.4785(7) 0.6213(7) 0.054(4) Uani 1 d
C15 C 1.0713(18) 0.4831(8) 0.6999(7) 0.069(5) Uani 1 d
C16 C 1.1382(17) 0.5597(10) 0.7219(7) 0.066(4) Uani 1 d
C17 C 1.0606(16) 0.6357(9) 0.6957(7) 0.065(4) Uani 1 d
C18 C 1.0481(16) 0.6336(8) 0.6201(7) 0.056(4) Uani 1 d
C19 C 0.9949(19) 0.4003(10) 0.5969(9) 0.068(5) Uani 1 d
C20 C 0.855(2) 0.3799(10) 0.6240(10) 0.099(7) Uani 1 d
C21 C 1.090(3) 0.3281(11) 0.6098(11) 0.116(8) Uani 1 d
C22 C 1.135(2) 0.7140(11) 0.7175(8) 0.106(7) Uani 1 d
C23 C 0.7264(13) 0.6138(7) 0.4973(6) 0.042(3) Uani 1 d
C24 C 0.6797(14) 0.6898(8) 0.4686(7) 0.063(3) Uani 1 d
H1N H 0.5175 0.4804 0.5910 0.080 Uiso 1 d
H2 H 0.3448 0.4987 0.8196 0.080 Uiso 1 d
H3N H 0.7181 0.5130 0.5119 0.080 Uiso 1 d
H31 H 0.5294 0.4835 0.9074 0.080 Uiso 1 d
H32 H 0.6260 0.4114 0.8542 0.080 Uiso 1 d
H41 H 0.3764 0.3762 0.8968 0.080 Uiso 1 d
H42 H 0.4981 0.3006 0.9222 0.080 Uiso 1 d
H5 H 0.5331 0.2704 0.8167 0.080 Uiso 1 d
H61 H 0.3405 0.2984 0.7361 0.080 Uiso 1 d
H62 H 0.2630 0.3538 0.7864 0.080 Uiso 1 d
H7 H 0.4981 0.5652 0.7382 0.080 Uiso 1 d
H81 H 0.4753 0.6477 0.8349 0.080 Uiso 1 d
H82 H 0.6127 0.6457 0.8260 0.080 Uiso 1 d
H83 H 0.5355 0.5893 0.8738 0.080 Uiso 1 d
H91 H 0.7461 0.5794 0.7579 0.080 Uiso 1 d
H92 H 0.7099 0.4933 0.7282 0.080 Uiso 1 d
H93 H 0.7119 0.5061 0.8079 0.080 Uiso 1 d
H101 H 0.3003 0.1785 0.8245 0.080 Uiso 1 d
H102 H 0.2632 0.2444 0.8798 0.080 Uiso 1 d
H103 H 0.3924 0.1935 0.8887 0.080 Uiso 1 d
H121 H 0.5477 0.2734 0.5287 0.080 Uiso 1 d
H122 H 0.3977 0.2560 0.5655 0.080 Uiso 1 d
H123 H 0.3960 0.3160 0.5012 0.080 Uiso 1 d
H14 H 1.1541 0.4631 0.6078 0.080 Uiso 1 d
H151 H 1.0053 0.4870 0.7126 0.080 Uiso 1 d
H152 H 1.1013 0.4134 0.7085 0.080 Uiso 1 d
H161 H 1.2435 0.5581 0.7064 0.080 Uiso 1 d
H162 H 1.1515 0.5415 0.7882 0.080 Uiso 1 d
H17 H 0.9764 0.6342 0.7167 0.080 Uiso 1 d
H181 H 0.9997 0.6808 0.6003 0.080 Uiso 1 d
H182 H 1.1422 0.6393 0.6030 0.080 Uiso 1 d
H19 H 0.9650 0.3920 0.5411 0.080 Uiso 1 d
H201 H 0.7943 0.4317 0.6231 0.080 Uiso 1 d
H202 H 0.8665 0.3579 0.6691 0.080 Uiso 1 d
H203 H 0.8190 0.3358 0.5969 0.080 Uiso 1 d
H211 H 1.0205 0.2671 0.6108 0.080 Uiso 1 d
H212 H 1.1549 0.3364 0.6488 0.080 Uiso 1 d
H213 H 1.1664 0.3253 0.5707 0.080 Uiso 1 d
H221 H 1.0914 0.7606 0.7007 0.080 Uiso 1 d
H222 H 1.1439 0.7157 0.7650 0.080 Uiso 1 d
H223 H 1.2271 0.7114 0.6981 0.080 Uiso 1 d
H241 H 0.5545 0.7000 0.4696 0.080 Uiso 1 d
H242 H 0.7376 0.7216 0.4740 0.080 Uiso 1 d
H243 H 0.6928 0.6800 0.4207 0.080 Uiso 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'
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'
Cl Cl 0.1484 0.1585 '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
N3 Re N1 83.7(4)
N3 Re Cl3 85.3(3)
N1 Re Cl3 92.0(4)
N3 Re Cl4 173.3(3)
N1 Re Cl4 89.8(3)
Cl3 Re Cl4 93.8(2)
N3 Re Cl2 93.3(3)
N1 Re Cl2 174.9(3)
Cl3 Re Cl2 91.72(16)
Cl4 Re Cl2 93.34(16)
N3 Re Cl1 88.3(3)
N1 Re Cl1 83.8(3)
Cl3 Re Cl1 172.67(18)
Cl4 Re Cl1 92.19(19)
Cl2 Re Cl1 92.07(16)
C11 O1 N2 111.9(9)
C23 O2 N4 111.5(9)
C11 N1 Re 135.8(9)
C1 N2 O1 110.1(10)
C23 N3 Re 138.0(9)
C13 N4 O2 112.3(11)
N2 C1 C2 118.8(12)
N2 C1 C6 126.1(12)
C2 C1 C6 115.1(10)
C1 C2 C7 113.9(11)
C1 C2 C3 106.6(11)
C7 C2 C3 113.5(13)
C4 C3 C2 111.9(14)
C3 C4 C5 113.0(12)
C4 C5 C6 109.9(12)
C4 C5 C10 113.2(12)
C6 C5 C10 110.1(13)
C1 C6 C5 109.9(11)
C8 C7 C2 109.6(12)
C8 C7 C9 110.3(15)
C2 C7 C9 115.0(14)
N1 C11 O1 123.2(12)
N1 C11 C12 127.9(11)
O1 C11 C12 108.9(11)
N4 C13 C14 116.9(13)
N4 C13 C18 125.8(13)
C14 C13 C18 117.2(11)
C13 C14 C19 115.2(13)
C13 C14 C15 110.3(11)
C19 C14 C15 113.5(11)
C16 C15 C14 112.0(11)
C15 C16 C17 111.3(11)
C18 C17 C22 109.7(13)
C18 C17 C16 110.9(12)
C22 C17 C16 109.8(12)
C17 C18 C13 111.8(11)
C14 C19 C20 116.2(15)
C14 C19 C21 111.1(14)
C20 C19 C21 109.1(15)
N3 C23 O2 122.0(11)
N3 C23 C24 126.4(12)
O2 C23 C24 111.6(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re N3 2.109(10)
Re N1 2.121(9)
Re Cl3 2.316(4)
Re Cl4 2.319(5)
Re Cl2 2.317(3)
Re Cl1 2.340(4)
O1 C11 1.350(13)
O1 N2 1.467(12)
O2 C23 1.344(15)
O2 N4 1.469(12)
N1 C11 1.259(15)
N2 C1 1.283(14)
N3 C23 1.257(15)
N4 C13 1.271(17)
C1 C2 1.503(18)
C1 C6 1.512(18)
C2 C7 1.54(2)
C2 C3 1.575(18)
C3 C4 1.49(2)
C4 C5 1.510(19)
C5 C6 1.525(18)
C5 C10 1.53(2)
C7 C8 1.52(2)
C7 C9 1.53(2)
C11 C12 1.491(17)
C13 C14 1.476(18)
C13 C18 1.516(19)
C14 C19 1.505(19)
C14 C15 1.576(19)
C15 C16 1.491(19)
C16 C17 1.56(2)
C17 C18 1.513(19)
C17 C22 1.55(2)
C19 C20 1.52(3)
C19 C21 1.54(2)
C23 C24 1.450(17)
