Cyclopentadiene-mediated hydride transfer from rhodium complexes.
Pitman, C. L.; Finster, O. N. L.; Miller, A. J. M.; Chemical communications (Cambridge, England) 52 (2016) 9105–9108; doi:10.1039/c6cc00575f

data_7118817
_publ_section_title
;
 Cyclopentadiene-mediated hydride transfer from rhodium complexes.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9105
_journal_page_last               9108
_journal_paper_doi               10.1039/c6cc00575f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C20 H24 Cl N2 Rh, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C21 H26 Cl3 N2 Rh'
_chemical_formula_weight         515.70
_chemical_name_systematic        (Cp*H)Rh(bpy)Cl
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5211(11)
_cell_length_b                   12.1599(6)
_cell_length_c                   7.8427(4)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.35
_cell_measurement_theta_min      3.93
_cell_volume                     2147.76(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18815
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.338
_diffrn_reflns_theta_min         3.926
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.921
_exptl_absorpt_correction_T_max  0.7647
_exptl_absorpt_correction_T_min  0.1358
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.1776.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dicloromethane/pentane'
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+2.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2191
_reflns_number_total             2224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00575f2.cif
_cod_data_source_block           x1511015
_cod_depositor_comments          'Adding full bibliography for 7118817.cif.'
_cod_database_code               7118817
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.166
_olex2_refinement_description
;
1. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H12A(0.5) H12B(0.5)
 Fixed U12: Rh1(0) Cl1(0) C1(0) C4(0) Cl2(0) Cl3(0) C12(0)
 Fixed U23: Rh1(0) Cl1(0) C1(0) C4(0) Cl2(0) Cl3(0) C12(0)
 Fixed Uiso: H1(0.021) H4A(0.034) H4B(0.034) H4C(0.034) H5A(0.034) H5B(0.034)
 H5C(0.034) H6A(0.032) H6B(0.032) H6C(0.032) H7(0.02) H8(0.022) H9(0.024)
 H10(0.021) H12A(0.059) H12B(0.059)
 Fixed X: H1(0.6227) H4A(0.5421) H4B(0.5468) H4C(0.4968) H5A(0.6272)
 H5B(0.5625) H5C(0.5719) H6A(0.4867) H6B(0.5182) H6C(0.4584) H7(0.6305)
 H8(0.6796) H9(0.7286) H10(0.7258) H12A(0.3057) H12B(0.3057)
 Fixed Y: Rh1(0.25) Cl1(0.25) C1(0.25) H1(0.25) C4(0.25) H4A(0.3188)
 H4B(0.1876) H4C(0.2436) H5A(0.47) H5B(0.4779) H5C(0.5095) H6A(0.3443)
 H6B(0.4495) H6C(0.4021) H7(0.5023) H8(0.6131) H9(0.5304) H10(0.3388) Cl2(0.25)
 Cl3(0.25) C12(0.25) H12A(0.1842) H12B(0.3158)
 Fixed Z: H1(0.5528) H4A(0.7274) H4B(0.7382) H4C(0.622) H5A(0.4547)
 H5B(0.5383) H5C(0.342) H6A(0.0334) H6B(0.1158) H6C(0.1976) H7(0.1075) H8(-
 0.087) H9(-0.3194) H10(-0.3485) H12A(0.5284) H12B(0.5284)
;
_shelx_res_checksum              83780
_shelx_hkl_checksum              97511
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'