#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/28/4122858.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_4122858
loop_
_publ_author_name
'Frank, René'
'Howell, James'
'Tirfoin, Rémi'
'Dange, Deepak'
'Jones, Cameron'
'Mingos, D Michael P'
'Aldridge, Simon'
_publ_section_title
;
 Circumventing redox chemistry: synthesis of transition metal boryl
 complexes from a boryl nucleophile by decarbonylation.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15730
_journal_page_last               15741
_journal_paper_doi               10.1021/ja508979x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C31 H36 B1 N2 O5 Re1'
_chemical_formula_sum            'C31 H36 B N2 O5 Re'
_chemical_formula_weight         713.65
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-04-17
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.23990(10)
_cell_length_b                   13.84230(10)
_cell_length_c                   20.2363(2)
_cell_measurement_reflns_used    12739
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     3148.49(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16429
_diffrn_reflns_theta_full        76.266
_diffrn_reflns_theta_max         76.266
_diffrn_reflns_theta_min         4.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.866
_exptl_absorpt_correction_T_max  0.39
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond_shape
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.53
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1776
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.0002469
_refine_ls_shift/su_mean         0.0000275
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 6.65P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0483
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0483
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                1775
_reflns_number_total             1786
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.67
_oxford_diffrn_Wilson_scale      0.28
_oxford_refine_ls_r_factor_ref   0.0183
_oxford_refine_ls_scale          1.951(10)
_oxford_reflns_number_all        1776
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '201JHRT14 in C m c m'
_cod_data_source_file            ja508979x_si_002.cif
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4122854--4122863.cif.
;
_cod_original_sg_symbol_H-M      'C m c m '
_cod_original_formula_sum        'C31 H36 B1 N2 O5 Re1'
_cod_database_code               4122858
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
-x,-y,z+1/2
x,y,-z+1/2
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2
x,-y,-z
-x,y,z
x+1/2,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Re1 Re 0.5000 0.181026(11) 0.7500 0.0223 1.0000 Uani S T
C2 C 0.5000 0.17683(18) 0.65034(16) 0.0271 1.0000 Uani S T
O3 O 0.5000 0.16539(16) 0.59556(11) 0.0360 1.0000 Uani S T
C4 C 0.5000 0.0382(3) 0.7500 0.0336 1.0000 Uani S T
O5 O 0.5000 -0.0445(2) 0.7500 0.0507 1.0000 Uani S T
C6 C 0.6763(3) 0.1967(2) 0.7500 0.0307 1.0000 Uani S T
O7 O 0.7762(2) 0.2084(2) 0.7500 0.0462 1.0000 Uani S T
B8 B 0.5000 0.3466(3) 0.7500 0.0193 1.0000 Uani S T
N9 N 0.5000 0.41225(16) 0.80566(11) 0.0238 1.0000 Uani S T
C10 C 0.5000 0.39370(18) 0.87542(13) 0.0222 1.0000 Uani S T
C11 C 0.60890(18) 0.38568(13) 0.90887(9) 0.0241 1.0000 Uani . .
C12 C 0.60652(19) 0.36971(16) 0.97703(10) 0.0282 1.0000 Uani . .
C13 C 0.500000(7) 0.3620(2) 1.01060(14) 0.0299 1.0000 Uani S T
C14 C 0.7273(2) 0.39516(16) 0.87328(11) 0.0313 1.0000 Uani . .
C15 C 0.8159(2) 0.3165(2) 0.89337(15) 0.0472 1.0000 Uani . .
C16 C 0.7806(3) 0.4953(2) 0.88525(16) 0.0585 1.0000 Uani . .
C17 C 0.500000(7) 0.5079(2) 0.78263(15) 0.0351 1.0000 Uani S T
H121 H 0.6770 0.3638 1.0002 0.0338 1.0000 Uiso R .
H131 H 0.5000 0.3515 1.0565 0.0369 1.0000 Uiso RS .
H141 H 0.7126 0.3870 0.8251 0.0368 1.0000 Uiso R .
H152 H 0.8854 0.3186 0.8648 0.0719 1.0000 Uiso R .
H151 H 0.8442 0.3275 0.9381 0.0719 1.0000 Uiso R .
H153 H 0.7805 0.2514 0.8911 0.0724 1.0000 Uiso R .
H163 H 0.8529 0.5046 0.8606 0.0886 1.0000 Uiso R .
H161 H 0.7965 0.5072 0.9310 0.0884 1.0000 Uiso R .
H162 H 0.7250 0.5446 0.8706 0.0889 1.0000 Uiso R .
H172 H 0.5000 0.5652 0.8067 0.0583 1.0000 Uiso RS .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Re -5.2083 5.8923 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861
10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 6_656 Re1 C6 6_656 90.179(8) yes
C2 6_656 Re1 C2 . 176.70(14) yes
C6 6_656 Re1 C2 . 90.179(8) yes
C2 6_656 Re1 C4 . 88.35(7) yes
C6 6_656 Re1 C4 . 96.24(9) yes
C2 . Re1 C4 . 88.35(7) yes
C2 6_656 Re1 C6 . 90.179(8) yes
C6 6_656 Re1 C6 . 167.51(18) yes
C2 . Re1 C6 . 90.179(8) yes
C4 . Re1 C6 . 96.24(9) yes
C2 6_656 Re1 B8 . 91.65(7) yes
C6 6_656 Re1 B8 . 83.76(9) yes
C2 . Re1 B8 . 91.65(7) yes
C4 . Re1 B8 . 179.995 yes
C6 . Re1 B8 . 83.76(9) yes
Re1 . C2 O3 . 173.5(2) yes
Re1 . C4 O5 . 179.990 yes
Re1 . C6 O7 . 178.0(3) yes
Re1 . B8 N9 6_656 128.89(16) yes
Re1 . B8 N9 . 128.89(16) yes
N9 6_656 B8 N9 . 102.2(3) yes
B8 . N9 C10 . 130.8(2) yes
B8 . N9 C17 . 109.5(2) yes
C10 . N9 C17 . 119.7(2) yes
N9 . C10 C11 14_655 119.26(12) yes
N9 . C10 C11 . 119.26(12) yes
C11 14_655 C10 C11 . 121.5(2) yes
C10 . C11 C12 . 118.17(19) yes
C10 . C11 C14 . 121.92(17) yes
C12 . C11 C14 . 119.91(19) yes
C11 . C12 C13 . 121.0(2) yes
C11 . C12 H121 . 119.9 no
C13 . C12 H121 . 119.1 no
C12 . C13 C12 14_655 120.3(3) yes
C12 . C13 H131 . 119.9 no
C12 14_655 C13 H131 . 119.9 no
C11 . C14 C15 . 112.50(19) yes
C11 . C14 C16 . 110.25(19) yes
C15 . C14 C16 . 110.4(2) yes
C11 . C14 H141 . 108.0 no
C15 . C14 H141 . 106.7 no
C16 . C14 H141 . 108.9 no
C14 . C15 H152 . 110.1 no
C14 . C15 H151 . 110.4 no
H152 . C15 H151 . 106.7 no
C14 . C15 H153 . 112.0 no
H152 . C15 H153 . 108.9 no
H151 . C15 H153 . 108.6 no
C14 . C16 H163 . 111.7 no
C14 . C16 H161 . 112.4 no
H163 . C16 H161 . 108.7 no
C14 . C16 H162 . 109.7 no
H163 . C16 H162 . 107.0 no
H161 . C16 H162 . 107.2 no
N9 . C17 C17 6_656 109.39(15) yes
N9 . C17 H172 . 129.1 no
C17 6_656 C17 H172 . 121.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 C2 6_656 2.018(3) yes
Re1 C6 6_656 1.994(3) yes
Re1 C2 . 2.018(3) yes
Re1 C4 . 1.977(4) yes
Re1 C6 . 1.994(3) yes
Re1 B8 . 2.292(4) yes
C2 O3 . 1.120(4) yes
C4 O5 . 1.144(6) yes
C6 O7 . 1.134(4) yes
B8 N9 6_656 1.447(3) yes
B8 N9 . 1.447(3) yes
N9 C10 . 1.435(3) yes
N9 C17 . 1.404(3) yes
C10 C11 14_655 1.403(2) yes
C10 C11 . 1.403(2) yes
C11 C12 . 1.397(3) yes
C11 C14 . 1.519(3) yes
C12 C13 . 1.381(3) yes
C12 H121 . 0.924 no
C13 H131 . 0.941 no
C14 C15 . 1.531(3) yes
C14 C16 . 1.530(3) yes
C14 H141 . 0.995 no
C15 H152 . 0.972 no
C15 H151 . 0.971 no
C15 H153 . 0.985 no
C16 H163 . 0.963 no
C16 H161 . 0.958 no
C16 H162 . 0.971 no
C17 C17 6_656 1.321(6) yes
C17 H172 . 0.930 no
