#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/56/4085692.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_4085692
loop_
_publ_author_name
'Böge, Matthias'
'Fowelin, Christian'
'Bednarski, Patrick'
'Heck, Jürgen'
_publ_section_title
;
 Diaminohexopyranosides as Ligands in Half-Sandwich Ruthenium(II),
 Rhodium(III), and Iridium(III) Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1507
_journal_paper_doi               10.1021/om5013117
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C24 H35 Cl N2 O4 Rh, B F4, C H2 Cl2, C H2 Cl2'
_chemical_formula_sum            'C26 H39 B Cl5 F4 N2 O4 Rh'
_chemical_formula_weight         810.56
_chemical_name_systematic
;
[T-4-S]-chlorido(methyl 
4,6-O-benzylidene-2,3-diamino-2,3-dideoxy-alpha-D-talopyranoside)-pentamethyl-pentahapto-cyclopentadienylrhodium(III) 
tetrafluoridoborate bisdichloromethane
;
_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                   12.73270(10)
_cell_length_b                   12.85280(10)
_cell_length_c                   20.42570(10)
_cell_measurement_reflns_used    17199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.6
_cell_measurement_theta_min      3.0
_cell_volume                     3342.68(4)
_computing_cell_refinement       'CrySalisPro (Agilent 2013)'
_computing_data_collection       'CrySalisPro (Agilent 2013)'
_computing_data_reduction        'CrySalisPro (Agilent 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Incoatec microfocus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            101905
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         37.50
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.7601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrySalisPro (Agilent 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.850
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.028(12)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         17199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0263P)²+1.8121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                16079
_reflns_number_total             17199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5013117_si_001.cif
_cod_data_source_block           46
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085684--4085692.cif.
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4085692
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.448300(8) 0.557623(8) 0.824923(5) 0.00987(2) Uani 1 1 d .
Cl1 Cl 0.43945(3) 0.42138(3) 0.743118(17) 0.01642(6) Uani 1 1 d .
N1 N 0.60606(9) 0.51076(10) 0.84507(6) 0.01224(19) Uani 1 1 d .
H1A H 0.6355 0.5544 0.8742 0.015 Uiso 1 1 calc R
H1B H 0.6068 0.4461 0.8620 0.015 Uiso 1 1 calc R
N2 N 0.53506(9) 0.64717(9) 0.75301(6) 0.01169(19) Uani 1 1 d .
H2A H 0.5064 0.6368 0.7133 0.014 Uiso 1 1 calc R
H2B H 0.5291 0.7153 0.7626 0.014 Uiso 1 1 calc R
O1 O 0.83854(8) 0.57024(8) 0.82166(5) 0.01370(16) Uani 1 1 d .
O2 O 0.67949(8) 0.72665(8) 0.84573(5) 0.01263(17) Uani 1 1 d .
O3 O 0.81983(8) 0.46830(9) 0.72787(5) 0.01517(19) Uani 1 1 d .
O4 O 0.84594(9) 0.77145(9) 0.88464(6) 0.0181(2) Uani 1 1 d .
C1 C 0.78219(11) 0.48852(11) 0.79126(7) 0.0133(2) Uani 1 1 d .
H1C H 0.7895 0.4254 0.8178 0.016 Uiso 1 1 calc R
C2 C 0.66545(11) 0.51300(10) 0.78292(7) 0.0116(2) Uani 1 1 d .
H2C H 0.6353 0.4600 0.7540 0.014 Uiso 1 1 calc R
C3 C 0.64908(10) 0.61892(11) 0.75047(7) 0.0112(2) Uani 1 1 d .
H3 H 0.6693 0.6126 0.7043 0.013 Uiso 1 1 calc R
C4 C 0.71768(11) 0.70256(11) 0.78143(7) 0.0124(2) Uani 1 1 d .
H4 H 0.7146 0.7654 0.7544 0.015 Uiso 1 1 calc R
C5 C 0.83141(11) 0.66638(11) 0.78608(7) 0.0140(2) Uani 1 1 d .
H5 H 0.8609 0.6577 0.7421 0.017 Uiso 1 1 calc R
C6 C 0.89407(11) 0.74637(12) 0.82378(9) 0.0181(2) Uani 1 1 d .
H6A H 0.9641 0.7196 0.8318 0.022 Uiso 1 1 calc R
H6B H 0.9006 0.8091 0.7976 0.022 Uiso 1 1 calc R
C7 C 0.92318(12) 0.42580(13) 0.72769(9) 0.0201(3) Uani 1 1 d .
H7A H 0.9712 0.4752 0.7464 0.030 Uiso 1 1 calc R
H7B H 0.9438 0.4106 0.6835 0.030 Uiso 1 1 calc R
H7C H 0.9242 0.3629 0.7531 0.030 Uiso 1 1 calc R
C8 C 0.74204(12) 0.80703(11) 0.87455(8) 0.0147(2) Uani 1 1 d .
H8 H 0.7431 0.8677 0.8455 0.018 Uiso 1 1 calc R
C9 C 0.69378(12) 0.83657(12) 0.93867(7) 0.0160(2) Uani 1 1 d .
C10 C 0.68785(14) 0.76467(13) 0.98955(8) 0.0207(3) Uani 1 1 d .
H10 H 0.7200 0.7000 0.9855 0.025 Uiso 1 1 calc R
C11 C 0.63347(16) 0.79024(15) 1.04645(9) 0.0252(3) Uani 1 1 d .
H11 H 0.6290 0.7423 1.0805 0.030 Uiso 1 1 calc R
C12 C 0.58594(16) 0.88703(16) 1.05259(9) 0.0261(3) Uani 1 1 d .
H12 H 0.5479 0.9030 1.0901 0.031 Uiso 1 1 calc R
C13 C 0.59512(15) 0.95985(14) 1.00290(9) 0.0244(3) Uani 1 1 d .
H13 H 0.5656 1.0256 1.0078 0.029 Uiso 1 1 calc R
C14 C 0.64885(13) 0.93438(13) 0.94540(8) 0.0193(3) Uani 1 1 d .
H14 H 0.6545 0.9828 0.9118 0.023 Uiso 1 1 calc R
C21 C 0.39828(11) 0.57811(11) 0.92513(7) 0.0131(2) Uani 1 1 d .
C22 C 0.33543(11) 0.50008(11) 0.89359(7) 0.0131(2) Uani 1 1 d .
C23 C 0.28076(10) 0.55008(12) 0.84001(7) 0.0137(2) Uani 1 1 d .
C24 C 0.31370(11) 0.65567(11) 0.83697(7) 0.0141(2) Uani 1 1 d .
C25 C 0.38668(11) 0.67411(11) 0.89017(7) 0.0135(2) Uani 1 1 d .
C26 C 0.46444(12) 0.56181(15) 0.98447(7) 0.0198(3) Uani 1 1 d .
H26A H 0.5218 0.6103 0.9842 0.030 Uiso 1 1 calc R
H26B H 0.4915 0.4921 0.9844 0.030 Uiso 1 1 calc R
H26C H 0.4227 0.5725 1.0230 0.030 Uiso 1 1 calc R
C27 C 0.32142(13) 0.38985(12) 0.91525(9) 0.0192(3) Uani 1 1 d .
H27A H 0.3854 0.3653 0.9347 0.029 Uiso 1 1 calc R
H27B H 0.3042 0.3473 0.8781 0.029 Uiso 1 1 calc R
H27C H 0.2657 0.3862 0.9468 0.029 Uiso 1 1 calc R
C28 C 0.20231(13) 0.50037(14) 0.79547(8) 0.0200(3) Uani 1 1 d .
H28A H 0.1327 0.5148 0.8110 0.030 Uiso 1 1 calc R
H28B H 0.2135 0.4265 0.7947 0.030 Uiso 1 1 calc R
H28C H 0.2104 0.5279 0.7521 0.030 Uiso 1 1 calc R
C29 C 0.27646(15) 0.73652(14) 0.79033(9) 0.0230(3) Uani 1 1 d .
H29A H 0.2461 0.7035 0.7526 0.034 Uiso 1 1 calc R
H29B H 0.3347 0.7790 0.7770 0.034 Uiso 1 1 calc R
H29C H 0.2245 0.7792 0.8113 0.034 Uiso 1 1 calc R
C30 C 0.43045(13) 0.77823(12) 0.90809(9) 0.0195(3) Uani 1 1 d .
H30A H 0.3759 0.8205 0.9267 0.029 Uiso 1 1 calc R
H30B H 0.4577 0.8116 0.8696 0.029 Uiso 1 1 calc R
H30C H 0.4859 0.7695 0.9395 0.029 Uiso 1 1 calc R
B1 B 0.60972(17) 1.23862(15) 0.91088(9) 0.0212(3) Uani 1 1 d .
F1 F 0.52925(11) 1.16804(11) 0.89632(7) 0.0406(3) Uani 1 1 d .
F2 F 0.64543(15) 1.28222(11) 0.85299(7) 0.0477(4) Uani 1 1 d .
F3 F 0.57053(10) 1.31983(11) 0.94909(7) 0.0350(3) Uani 1 1 d .
F4 F 0.69055(10) 1.19001(10) 0.94358(7) 0.0351(3) Uani 1 1 d .
C41 C 0.79301(18) 0.39201(16) 1.02741(9) 0.0282(4) Uani 1 1 d .
H41A H 0.7545 0.3317 1.0119 0.034 Uiso 1 1 calc R
H41B H 0.8598 0.3681 1.0446 0.034 Uiso 1 1 calc R
Cl2 Cl 0.81558(4) 0.47821(4) 0.96104(2) 0.02860(9) Uani 1 1 d .
Cl3 Cl 0.72163(6) 0.45271(6) 1.09019(3) 0.04712(15) Uani 1 1 d .
C42 C 1.0552(2) 0.71701(17) 0.59092(10) 0.0338(4) Uani 1 1 d .
H42A H 1.0323 0.6886 0.5493 0.041 Uiso 1 1 calc R
H42B H 1.1217 0.7522 0.5838 0.041 Uiso 1 1 calc R
Cl4 Cl 0.96198(5) 0.80742(5) 0.61883(3) 0.04356(13) Uani 1 1 d .
Cl5 Cl 1.07343(5) 0.61525(6) 0.64690(4) 0.05041(17) Uani 1 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Rh Rh -1.1178 0.9187 '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
N1 Rh1 C22 114.05(5)
N1 Rh1 C24 153.63(5)
C22 Rh1 C24 65.83(5)
N1 Rh1 C25 114.80(5)
C22 Rh1 C25 65.78(5)
C24 Rh1 C25 39.45(6)
N1 Rh1 C23 152.77(5)
C22 Rh1 C23 39.37(5)
C24 Rh1 C23 38.62(6)
C25 Rh1 C23 65.32(5)
N1 Rh1 C21 97.41(5)
C22 Rh1 C21 39.01(5)
C24 Rh1 C21 65.38(5)
C25 Rh1 C21 38.83(5)
C23 Rh1 C21 65.07(5)
N1 Rh1 N2 78.53(4)
C22 Rh1 N2 165.81(5)
C24 Rh1 N2 99.97(5)
C25 Rh1 N2 103.64(5)
C23 Rh1 N2 128.63(5)
C21 Rh1 N2 136.67(5)
N1 Rh1 Cl1 88.44(4)
C22 Rh1 Cl1 99.85(4)
C24 Rh1 Cl1 117.86(4)
C25 Rh1 Cl1 155.88(4)
C23 Rh1 Cl1 91.15(4)
C21 Rh1 Cl1 136.72(4)
N2 Rh1 Cl1 86.57(3)
C2 N1 Rh1 108.06(8)
C3 N2 Rh1 112.87(8)
C1 O1 C5 112.61(11)
C8 O2 C4 110.11(11)
C1 O3 C7 112.84(12)
C8 O4 C6 110.41(12)
O3 C1 O1 111.63(12)
O3 C1 C2 105.48(12)
O1 C1 C2 112.89(11)
N1 C2 C3 108.67(11)
N1 C2 C1 113.43(12)
C3 C2 C1 111.36(11)
N2 C3 C4 111.75(11)
N2 C3 C2 109.46(11)
C4 C3 C2 111.75(11)
O2 C4 C3 109.77(11)
O2 C4 C5 109.33(11)
C3 C4 C5 110.83(12)
O1 C5 C6 107.10(12)
O1 C5 C4 110.74(11)
C6 C5 C4 109.00(12)
O4 C6 C5 111.82(12)
O4 C8 O2 110.30(12)
O4 C8 C9 109.80(12)
O2 C8 C9 108.35(12)
C14 C9 C10 120.32(15)
C14 C9 C8 119.07(14)
C10 C9 C8 120.48(14)
C11 C10 C9 119.56(16)
C12 C11 C10 120.23(17)
C13 C12 C11 120.13(17)
C12 C13 C14 119.90(17)
C9 C14 C13 119.79(16)
C25 C21 C22 108.68(12)
C25 C21 C26 125.75(14)
C22 C21 C26 125.56(14)
C25 C21 Rh1 70.31(8)
C22 C21 Rh1 69.75(8)
C26 C21 Rh1 125.93(10)
C21 C22 C23 107.29(12)
C21 C22 C27 126.57(13)
C23 C22 C27 125.95(14)
C21 C22 Rh1 71.24(8)
C23 C22 Rh1 70.97(8)
C27 C22 Rh1 126.99(10)
C24 C23 C22 108.36(12)
C24 C23 C28 125.35(14)
C22 C23 C28 126.28(14)
C24 C23 Rh1 70.08(8)
C22 C23 Rh1 69.66(8)
C28 C23 Rh1 126.37(10)
C23 C24 C25 108.21(12)
C23 C24 C29 126.93(14)
C25 C24 C29 124.77(14)
C23 C24 Rh1 71.30(8)
C25 C24 Rh1 70.68(8)
C29 C24 Rh1 126.35(11)
C21 C25 C24 107.39(12)
C21 C25 C30 127.59(14)
C24 C25 C30 124.68(14)
C21 C25 Rh1 70.86(8)
C24 C25 Rh1 69.86(8)
C30 C25 Rh1 129.67(10)
F4 B1 F2 110.63(18)
F4 B1 F3 109.59(16)
F2 B1 F3 106.99(16)
F4 B1 F1 110.86(15)
F2 B1 F1 108.71(17)
F3 B1 F1 109.98(17)
Cl3 C41 Cl2 111.39(12)
Cl5 C42 Cl4 111.80(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 N1 2.1371(12)
Rh1 C22 2.1400(14)
Rh1 C24 2.1415(14)
Rh1 C25 2.1525(14)
Rh1 C23 2.1576(13)
Rh1 C21 2.1597(14)
Rh1 N2 2.1687(12)
Rh1 Cl1 2.4230(3)
N1 C2 1.4779(18)
N2 C3 1.4974(17)
O1 C1 1.4154(17)
O1 C5 1.4364(18)
O2 C8 1.4311(17)
O2 C4 1.4343(18)
O3 C1 1.4050(18)
O3 C7 1.4249(18)
O4 C8 1.4148(19)
O4 C6 1.423(2)
C1 C2 1.5289(19)
C2 C3 1.5284(19)
C3 C4 1.523(2)
C4 C5 1.524(2)
C5 C6 1.512(2)
C8 C9 1.496(2)
C9 C14 1.388(2)
C9 C10 1.393(2)
C10 C11 1.392(3)
C11 C12 1.389(3)
C12 C13 1.386(3)
C13 C14 1.398(2)
C21 C25 1.433(2)
C21 C22 1.436(2)
C21 C26 1.491(2)
C22 C23 1.448(2)
C22 C27 1.495(2)
C23 C24 1.422(2)
C23 C28 1.495(2)
C24 C25 1.449(2)
C24 C29 1.487(2)
C25 C30 1.495(2)
B1 F4 1.377(2)
B1 F2 1.385(2)
B1 F3 1.396(2)
B1 F1 1.400(2)
C41 Cl3 1.755(2)
C41 Cl2 1.774(2)
C42 Cl5 1.753(2)
C42 Cl4 1.756(2)
