Halide-Bridged Binuclear HX-Splitting Catalysts.
Powers, David C.; Hwang, Seung Jun; Zheng, Shao-Liang; Nocera, Daniel G.; Inorganic chemistry 53 (2014) 9122–9128; doi:10.1021/ic501136m

data_4340873
_publ_section_title
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 Halide-Bridged Binuclear HX-Splitting Catalysts.
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_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9122
_journal_page_last               9128
_journal_paper_doi               10.1021/ic501136m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C16.5 H19 Cl1.5 F12 N1.5 O4.5 P2 Rh'
_chemical_formula_weight         756.36
_chemical_name_common            Rh2Cl3H(tfepma)2(4-MeO-C6H4NC)
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.7710(6)
_cell_angle_beta                 86.0740(6)
_cell_angle_gamma                68.9300(5)
_cell_formula_units_Z            4
_cell_length_a                   11.3961(4)
_cell_length_b                   15.6785(6)
_cell_length_c                   17.1337(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2675.01(17)
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39904
_diffrn_reflns_theta_full        25.1066
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.020
_exptl_crystal_density_diffrn    1.8779
_exptl_crystal_F_000             1490.4663
_refine_diff_density_max         0.8730
_refine_diff_density_min         -0.6270
_refine_diff_density_rms         0.1036
_refine_ls_d_res_high            0.8375
_refine_ls_d_res_low             16.0441
_refine_ls_goodness_of_fit_ref   1.0512
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    85
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9526
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0505
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.0527
_refine_ls_shift/su_mean         0.0009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+3.1402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8086
_reflns_number_total             9526
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic501136m_si_002.cif
_cod_data_source_block           Rh2Cl3H(tfepma)2(4-MeO-C6H4NC)
_cod_depositor_comments
'Adding full bibliography for 4340872--4340876.cif.'
_cod_original_formula_sum        'C16.50 H19 Cl1.50 F12 N1.50 O4.50 P2 Rh'
_cod_database_code               4340873
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H5a,H5b} of C5, {H7a,H7b} of C7, {H1a,H1b} of C1, {H3a,H3b} of C3, {H10a,
  H10b,H10c,H10d} of C10, {H12a,H12b} of C12, {H14a,H14b} of C14, {H16a,H16b}
  of C16, H21 of C21, H22 of C22, H24 of C24, H25 of C25, H7T of C7T, H6T of
  C6T, H3S of C3S, H1 of Rh1, H3T of C3T, H4T of C4T, H5T of C5T, H4S of C4S,
  H5S of C5S, H6S of C6S, H7S of C7S
 At 1.5 times of:
  {H18a,H18b,H18c} of C18, {H26a,H26b,H26c} of C26, {H1Sa,H1Sb,H1Sc} of C1S,
  {H1Ta,H1Tb,H1Tc} of C1T, {H9a,H9b,H9c} of C9
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C10 ~ C11 ~ C11A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F13) = Uanis(F13A) = Uanis(F14) = Uanis(F14A) = Uanis(F15) = Uanis(F15A)
Uanis(C10) = Uanis(C11) = Uanis(C11A)
Uanis(C1S) = Uanis(C1T)
Uanis(C2T) = Uanis(C3T) = Uanis(C4T) = Uanis(C5T) = Uanis(C6T) = Uanis(C7T) = Uanis(C2S) = Uanis(C3S) = Uanis(C4S) = Uanis(C5S) = Uanis(C6S) = Uanis(C7S)
4. Others
 Sof(H10a)=Sof(H10b)=1-Sof(H10b)=1-Sof(H10b)=Sof(C11)=Sof(F13)=Sof(F14)=
 Sof(F15)=1-Sof(H10b)=1-Sof(H10b)=1-Sof(H10b)=1-Sof(H10b)
 Sof(C1S)=Sof(H1Sa)=Sof(H1Sb)=Sof(H1Sc)=Sof(C2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=
 Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=Sof(C7S)=Sof(H7S)=1-Sof(H1Sa)=1-
 Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-
 Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-Sof(H1Sa)=1-
 Sof(H1Sa)=1-Sof(H1Sa)
5.a Riding coordinates:
 Rh1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C5(H5a,H5b), C7(H7a,H7b), C10(H10a,H10b), C10(H10c,
 H10d), C12(H12a,H12b), C14(H14a,H14b), C16(H16a,H16b)
5.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C24(H24), C25(H25), C3S(H3S), C4S(H4S), C5S(H5S),
 C6S(H6S), C7S(H7S), C7T(H7T), C6T(H6T), C5T(H5T), C4T(H4T), C3T(H3T)
5.d Fitted hexagon refined as free rotating group:
 C2S(C3S,C4S,C5S,C6S,C7S), C2T(C7T,C6T,C5T,C4T,C3T)
5.e Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C18(H18a,H18b,H18c), C26(H26a,H26b,H26c), C1S(H1Sa,H1Sb,
 H1Sc), C1T(H1Ta,H1Tb,H1Tc)
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