#------------------------------------------------------------------------------
#$Date: 2016-11-08 22:08:11 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040686.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_7040686
loop_
_publ_author_name
'Iturmendi, Amaia'
'Sanz Miguel, Pablo J.'
'Popoola, Saheed A.'
'Al-Saadi, Abdulaziz A'
'Iglesias, Manuel'
'Oro, Luis A.'
_publ_section_title
;
 Dimethylphosphinate bridged binuclear Rh(i) catalysts for the
 alkoxycarbonylation of aromatic C-H bonds.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16955
_journal_page_last               16965
_journal_paper_doi               10.1039/c6dt03010f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C32 H38 O8 P4 Rh2'
_chemical_formula_weight         880.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-27 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9476(11)
_cell_length_b                   9.3438(5)
_cell_length_c                   20.4044(11)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.44
_cell_volume                     3575.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21038
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.597
_diffrn_reflns_theta_min         2.123
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0274P)²+5.3938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3740
_reflns_number_total             4308
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03010f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7040683--7040686.cif.'
_cod_database_code               7040686
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.803
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Rh1 Rh 0.41675(2) 0.00246(2) 0.66325(2) 0.01848(5) Uani 1 1 d . .
C11 C 0.33505(11) 0.0720(2) 0.66870(10) 0.0245(4) Uani 1 1 d . .
O12 O 0.28197(8) 0.11368(18) 0.67200(8) 0.0365(4) Uani 1 1 d . .
P20 P 0.56212(3) -0.18548(5) 0.69531(3) 0.02278(11) Uani 1 1 d . .
O21 O 0.50967(7) -0.07510(14) 0.65193(7) 0.0241(3) Uani 1 1 d . .
O22 O 0.58061(8) -0.17626(14) 0.77361(7) 0.0242(3) Uani 1 1 d . .
C23 C 0.64231(12) -0.1671(3) 0.67493(12) 0.0361(5) Uani 1 1 d . .
H231 H 0.6317 -0.1827 0.6249 0.054 Uiso 1 1 calc R U
H232 H 0.6773 -0.2380 0.7013 0.054 Uiso 1 1 calc R U
H233 H 0.6618 -0.0707 0.6874 0.054 Uiso 1 1 calc R U
C24 C 0.52854(14) -0.3614(2) 0.66871(11) 0.0348(5) Uani 1 1 d . .
H241 H 0.5193 -0.3727 0.6186 0.052 Uiso 1 1 calc R U
H242 H 0.4841 -0.3755 0.6784 0.052 Uiso 1 1 calc R U
H243 H 0.5638 -0.4324 0.6945 0.052 Uiso 1 1 calc R U
P30 P 0.41713(3) 0.17111(5) 0.58847(2) 0.01853(10) Uani 1 1 d . .
C31 C 0.50458(10) 0.24582(19) 0.59953(10) 0.0204(4) Uani 1 1 d . .
C32 C 0.51591(11) 0.3136(2) 0.54329(10) 0.0239(4) Uani 1 1 d . .
H32 H 0.4781 0.3201 0.4999 0.029 Uiso 1 1 calc R U
C33 C 0.58195(11) 0.3715(2) 0.55017(11) 0.0282(4) Uani 1 1 d . .
H33 H 0.5894 0.4161 0.5114 0.034 Uiso 1 1 calc R U
C34 C 0.63700(11) 0.3643(2) 0.61366(12) 0.0311(5) Uani 1 1 d . .
H34 H 0.6821 0.4048 0.6185 0.037 Uiso 1 1 calc R U
C35 C 0.62625(11) 0.2980(2) 0.67022(11) 0.0295(4) Uani 1 1 d . .
H35 H 0.6641 0.2932 0.7137 0.035 Uiso 1 1 calc R U
C36 C 0.56008(10) 0.2384(2) 0.66326(10) 0.0245(4) Uani 1 1 d . .
H36 H 0.5528 0.1928 0.7019 0.029 Uiso 1 1 calc R U
C41 C 0.36323(10) 0.3307(2) 0.58067(10) 0.0214(4) Uani 1 1 d . .
C42 C 0.31504(10) 0.3768(2) 0.51736(10) 0.0237(4) Uani 1 1 d . .
H42 H 0.3085 0.3224 0.4763 0.028 Uiso 1 1 calc R U
C43 C 0.27616(11) 0.5026(2) 0.51385(12) 0.0280(4) Uani 1 1 d . .
H43 H 0.2427 0.5331 0.4707 0.034 Uiso 1 1 calc R U
C44 C 0.28654(12) 0.5820(2) 0.57323(13) 0.0349(5) Uani 1 1 d . .
H44 H 0.2608 0.6686 0.5707 0.042 Uiso 1 1 calc R U
C45 C 0.33405(13) 0.5371(3) 0.63665(13) 0.0417(6) Uani 1 1 d . .
H45 H 0.3408 0.5924 0.6775 0.050 Uiso 1 1 calc R U
C46 C 0.37176(12) 0.4109(2) 0.64030(12) 0.0342(5) Uani 1 1 d . .
H46 H 0.4037 0.3790 0.6840 0.041 Uiso 1 1 calc R U
O51 O 0.38888(7) 0.12068(14) 0.50793(7) 0.0236(3) Uani 1 1 d . .
C52 C 0.40386(12) -0.0248(2) 0.49266(11) 0.0295(5) Uani 1 1 d . .
H521 H 0.3906 -0.0369 0.4421 0.044 Uiso 1 1 calc R U
H522 H 0.3762 -0.0914 0.5105 0.044 Uiso 1 1 calc R U
H523 H 0.4548 -0.0444 0.5150 0.044 Uiso 1 1 calc R U
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'
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C11 Rh1 O21 177.24(7) . .
C11 Rh1 O22 94.80(7) . 2_656
O21 Rh1 O22 87.35(5) . 2_656
C11 Rh1 P30 90.07(7) . .
O21 Rh1 P30 87.63(4) . .
O22 Rh1 P30 172.97(4) 2_656 .
O12 C11 Rh1 178.47(18) . .
O22 P20 O21 116.59(8) . .
O22 P20 C24 107.69(9) . .
O21 P20 C24 109.55(10) . .
O22 P20 C23 108.85(10) . .
O21 P20 C23 106.96(9) . .
C24 P20 C23 106.79(12) . .
P20 O21 Rh1 129.48(8) . .
P20 O22 Rh1 129.71(8) . 2_656
P20 C23 H231 109.5 . .
P20 C23 H232 109.5 . .
H231 C23 H232 109.5 . .
P20 C23 H233 109.5 . .
H231 C23 H233 109.5 . .
H232 C23 H233 109.5 . .
P20 C24 H241 109.5 . .
P20 C24 H242 109.5 . .
H241 C24 H242 109.5 . .
P20 C24 H243 109.5 . .
H241 C24 H243 109.5 . .
H242 C24 H243 109.5 . .
O51 P30 C41 99.18(8) . .
O51 P30 C31 103.04(8) . .
C41 P30 C31 102.13(8) . .
O51 P30 Rh1 114.52(5) . .
C41 P30 Rh1 120.60(6) . .
C31 P30 Rh1 114.78(6) . .
C36 C31 C32 119.38(18) . .
C36 C31 P30 121.33(15) . .
C32 C31 P30 119.28(15) . .
C33 C32 C31 120.57(19) . .
C33 C32 H32 119.7 . .
C31 C32 H32 119.7 . .
C34 C33 C32 119.94(19) . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C33 C34 C35 120.05(19) . .
C33 C34 H34 120.0 . .
C35 C34 H34 120.0 . .
C34 C35 C36 120.1(2) . .
C34 C35 H35 119.9 . .
C36 C35 H35 119.9 . .
C31 C36 C35 119.93(19) . .
C31 C36 H36 120.0 . .
C35 C36 H36 120.0 . .
C46 C41 C42 119.11(18) . .
C46 C41 P30 118.33(15) . .
C42 C41 P30 122.54(15) . .
C41 C42 C43 120.30(19) . .
C41 C42 H42 119.9 . .
C43 C42 H42 119.9 . .
C44 C43 C42 119.7(2) . .
C44 C43 H43 120.2 . .
C42 C43 H43 120.2 . .
C43 C44 C45 120.7(2) . .
C43 C44 H44 119.7 . .
C45 C44 H44 119.7 . .
C44 C45 C46 119.6(2) . .
C44 C45 H45 120.2 . .
C46 C45 H45 120.2 . .
C45 C46 C41 120.6(2) . .
C45 C46 H46 119.7 . .
C41 C46 H46 119.7 . .
C52 O51 P30 117.81(12) . .
O51 C52 H521 109.5 . .
O51 C52 H522 109.5 . .
H521 C52 H522 109.5 . .
O51 C52 H523 109.5 . .
H521 C52 H523 109.5 . .
H522 C52 H523 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C11 1.793(2) .
Rh1 O21 2.0749(13) .
Rh1 O22 2.0988(13) 2_656
Rh1 P30 2.1953(5) .
C11 O12 1.151(2) .
P20 O22 1.5148(14) .
P20 O21 1.5202(14) .
P20 C24 1.788(2) .
P20 C23 1.793(2) .
O22 Rh1 2.0988(13) 2_656
C23 H231 0.9800 .
C23 H232 0.9800 .
C23 H233 0.9800 .
C24 H241 0.9800 .
C24 H242 0.9800 .
C24 H243 0.9800 .
P30 O51 1.6154(14) .
P30 C41 1.8133(19) .
P30 C31 1.8202(19) .
C31 C36 1.393(3) .
C31 C32 1.395(3) .
C32 C33 1.386(3) .
C32 H32 0.9500 .
C33 C34 1.385(3) .
C33 H33 0.9500 .
C34 C35 1.390(3) .
C34 H34 0.9500 .
C35 C36 1.395(3) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C41 C46 1.389(3) .
C41 C42 1.390(3) .
C42 C43 1.397(3) .
C42 H42 0.9500 .
C43 C44 1.375(3) .
C43 H43 0.9500 .
C44 C45 1.384(3) .
C44 H44 0.9500 .
C45 C46 1.387(3) .
C45 H45 0.9500 .
C46 H46 0.9500 .
O51 C52 1.448(2) .
C52 H521 0.9800 .
C52 H522 0.9800 .
C52 H523 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O22 P20 O21 Rh1 -41.62(14) .
C24 P20 O21 Rh1 80.96(13) .
C23 P20 O21 Rh1 -163.65(12) .
O21 P20 O22 Rh1 -29.29(14) 2_656
C24 P20 O22 Rh1 -152.83(12) 2_656
C23 P20 O22 Rh1 91.74(13) 2_656
O51 P30 C31 C36 -148.41(15) .
C41 P30 C31 C36 109.04(16) .
Rh1 P30 C31 C36 -23.23(18) .
O51 P30 C31 C32 32.50(17) .
C41 P30 C31 C32 -70.05(17) .
Rh1 P30 C31 C32 157.68(13) .
C36 C31 C32 C33 0.9(3) .
P30 C31 C32 C33 179.99(15) .
C31 C32 C33 C34 -1.1(3) .
C32 C33 C34 C35 0.6(3) .
C33 C34 C35 C36 0.0(3) .
C32 C31 C36 C35 -0.3(3) .
P30 C31 C36 C35 -179.35(15) .
C34 C35 C36 C31 -0.2(3) .
O51 P30 C41 C46 -179.28(17) .
C31 P30 C41 C46 -73.71(18) .
Rh1 P30 C41 C46 54.98(18) .
O51 P30 C41 C42 -0.55(17) .
C31 P30 C41 C42 105.03(17) .
Rh1 P30 C41 C42 -126.28(15) .
C46 C41 C42 C43 0.4(3) .
P30 C41 C42 C43 -178.29(15) .
C41 C42 C43 C44 1.0(3) .
C42 C43 C44 C45 -1.3(3) .
C43 C44 C45 C46 0.2(4) .
C44 C45 C46 C41 1.2(4) .
C42 C41 C46 C45 -1.5(3) .
P30 C41 C46 C45 177.3(2) .
C41 P30 O51 C52 -163.71(14) .
C31 P30 O51 C52 91.46(15) .
Rh1 P30 O51 C52 -33.88(15) .
