Carbide complexes as π-acceptor ligands
Reinholdt, Anders; Vibenholt, Johan E.; Morsing, Thorbjørn J.; Schau-Magnussen, Magnus; Reeler, Nini E. A.; Bendix, Jesper; Chem. Sci. 6 (2015) 5815–; doi:10.1039/C5SC02077H

data_1521284
_publ_section_title
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 Carbide complexes as \p-acceptor ligands
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5815
_journal_paper_doi               10.1039/C5SC02077H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C45 H78 Cl3 P2 Rh Ru, C H2 Cl2'
_chemical_formula_sum            'C46 H80 Cl5 P2 Rh Ru'
_chemical_formula_weight         1076.27
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-26 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                78.174(4)
_cell_angle_beta                 75.183(12)
_cell_angle_gamma                75.241(8)
_cell_formula_units_Z            2
_cell_length_a                   10.9350(12)
_cell_length_b                   12.9950(5)
_cell_length_c                   18.693(3)
_cell_measurement_temperature    122(2)
_cell_volume                     2455.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  diffractometer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54616
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.851
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         10014
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0194
_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/[\s^2^(Fo^2^)+(0.0170P)^2^+2.1830P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9186
_reflns_number_total             10014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02077h2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 1521279--1521290.cif.'
_cod_database_code               1521284
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-C2AA \\sim Cl2A-C2AB \\sim Cl1-C2AA \\sim Cl1A-C2AB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C7)
Uanis(C2AB) = Uanis(C2AA)
4. Others
 Sof(C2AB)=Sof(H2AC)=Sof(H2AD)=Sof(Cl2A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H33A(0.5) H33(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) C47(0.5) H47(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) H4B(0.5) H4A(0.5) C6(0.5) H6(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10(0.5) C12(0.5) H12A(0.5) H12B(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) C3(0.5) H3(0.5)
5.a Riding coordinates:
 C33(H33A), C33(H33), C47(H47), C4(H4B), C4(H4A), C6(H6), C10(H10), C3(H3)
5.b Ternary CH refined with riding coordinates:
 C15(H15), C22(H22), C25(H25), C27(H27), C32(H32), C36(H36)
5.c Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C11(H11A,H11B), C1AA(H1AA,H1AB), C13(H13A,H13B), C14(H14A,
 H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
  C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C34(H34A,H34B), C35(H35A,
 H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C9(H9A,H9B), C12(H12A,H12B), C2AA(H2AA,H2AB), C3AA(H3AA,
 H3AB), C7(H7A,H7B), C2AB(H2AC,H2AD)
;
_shelx_res_checksum              32669