Incorporation of Pendant Bases into Rh(diphosphine)2 Complexes: Synthesis, Thermodynamic Studies, And Catalytic CO2 Hydrogenation Activity of [Rh(P2N2)2](+) Complexes.
Lilio, Alyssia M.; Reineke, Mark H.; Moore, Curtis E.; Rheingold, Arnold L.; Takase, Michael K.; Kubiak, Clifford P.; Journal of the American Chemical Society 137 (2015) 8251–8260; doi:10.1021/jacs.5b04291

data_4123901
_publ_section_title
;
 Incorporation of Pendant Bases into Rh(diphosphine)2 Complexes:
 Synthesis, Thermodynamic Studies, And Catalytic CO2 Hydrogenation
 Activity of [Rh(P2N2)2](+) Complexes.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8251
_journal_page_last               8260
_journal_paper_doi               10.1021/jacs.5b04291
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C60 H65 N4 P4 Rh'
_chemical_formula_sum            'C60 H65 N4 P4 Rh'
_chemical_formula_weight         1068.95
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4866)
;
_cell_angle_alpha                96.498(2)
_cell_angle_beta                 90.811(3)
_cell_angle_gamma                100.226(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0163(7)
_cell_length_b                   14.2416(9)
_cell_length_c                   18.7726(12)
_cell_measurement_reflns_used    9574
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.13
_cell_measurement_theta_min      2.31
_cell_volume                     2616.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KAPPA APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            159545
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.387
_diffrn_reflns_theta_min         1.463
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         25463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.9758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21328
_reflns_number_total             25463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04291_si_002.cif
_cod_data_source_block           A14441
_cod_database_code               4123901
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.009) H12(0.021) H13(0.026) H14(0.032) H15(0.04) H16(0.031)
 H1A(0.014) H1B(0.014) H5A(0.016) H5B(0.016) H22(0.024) H23(0.03) H24(0.031)
 H25(0.029) H26(0.023) H2A(0.015) H2B(0.015) H32(0.019) H33(0.022) H34(0.024)
 H35(0.028) H36(0.023) H3A(0.016) H3B(0.016) H6A(0.022) H6B(0.022) H42(0.022)
 H43(0.026) H44(0.029) H45(0.028) H46(0.024) H4A(0.015) H4B(0.015) H62(0.017)
 H63(0.019) H64(0.019) H65(0.018) H66(0.015) H51A(0.016) H51B(0.016) H72(0.018)
 H73(0.023) H74(0.027) H75(0.028) H76(0.022) H55A(0.018) H55B(0.018)
 H52A(0.015) H52B(0.015) H82(0.016) H83(0.021) H84(0.023) H85(0.021) H86(0.016)
 H53A(0.014) H53B(0.014) H56A(0.019) H56B(0.019) H92(0.024) H93(0.034)
 H94(0.036) H95(0.033) H96(0.025) H54A(0.016) H54B(0.016)
 Fixed X: H12(0.5181) H13(0.499) H14(0.6564) H15(0.8233) H16(0.8418)
 H1A(0.9193) H1B(0.8432) H5A(1.1017) H5B(1.0942) H22(1.0431) H23(1.0783)
 H24(1.1466) H25(1.1811) H26(1.1408) H2A(0.8169) H2B(0.8857) H32(0.8406)
 H33(0.8283) H34(0.6287) H35(0.4415) H36(0.4543) H3A(0.4586) H3B(0.5608)
 H6A(0.5376) H6B(0.4269) H42(0.3953) H43(0.478) H44(0.7117) H45(0.8624)
 H46(0.7797) H4A(0.5844) H4B(0.4769) H62(0.3404) H63(0.1259) H64(0.016)
 H65(0.1174) H66(0.331) H51A(0.6297) H51B(0.5603) H72(0.7868) H73(0.8502)
 H74(0.9391) H75(0.957) H76(0.8872) H55A(0.8687) H55B(0.7151) H52A(0.945)
 H52B(0.8695) H82(1.1001) H83(1.3044) H84(1.3105) H85(1.1088) H86(0.9037)
 H53A(0.8388) H53B(0.8187) H56A(0.6112) H56B(0.4989) H92(0.7451) H93(0.8534)
 H94(0.8438) H95(0.7305) H96(0.6247) H54A(0.5711) H54B(0.456)
 Fixed Y: H12(0.4911) H13(0.6243) H14(0.6728) H15(0.5815) H16(0.4474)
 H1A(0.3783) H1B(0.2777) H5A(0.3285) H5B(0.2549) H22(0.2506) H23(0.126) H24(-
 0.0104) H25(-0.0223) H26(0.1005) H2A(0.134) H2B(0.143) H32(0.1226) H33(-
 0.0034) H34(-0.1175) H35(-0.1039) H36(0.0196) H3A(0.126) H3B(0.0522)
 H6A(0.0367) H6B(0.1051) H42(0.1394) H43(0.1884) H44(0.2212) H45(0.201)
 H46(0.1467) H4A(0.2822) H4B(0.2654) H62(0.3619) H63(0.2744) H64(0.157)
 H65(0.1299) H66(0.2184) H51A(0.2392) H51B(0.3028) H72(0.1864) H73(0.0576)
 H74(0.0806) H75(0.2307) H76(0.3577) H55A(0.4261) H55B(0.3902) H52A(0.3999)
 H52B(0.2975) H82(0.3922) H83(0.4489) H84(0.5557) H85(0.6015) H86(0.5424)
 H53A(0.5926) H53B(0.5425) H56A(0.5454) H56B(0.5912) H92(0.656) H93(0.8116)
 H94(0.94) H95(0.9111) H96(0.756) H54A(0.4833) H54B(0.5004)
 Fixed Z: H12(0.8536) H13(0.9353) H14(1.031) H15(1.05) H16(0.9692) H1A(0.8753)
 H1B(0.8972) H5A(0.83) H5B(0.7588) H22(0.9489) H23(1.0133) H24(0.9559)
 H25(0.8325) H26(0.767) H2A(0.8081) H2B(0.7322) H32(0.617) H33(0.525)
 H34(0.503) H35(0.5738) H36(0.6681) H3A(0.7839) H3B(0.789) H6A(0.9061)
 H6B(0.9164) H42(1.0404) H43(1.1583) H44(1.184) H45(1.0916) H46(0.9744)
 H4A(0.9358) H4B(0.8698) H62(0.4977) H63(0.4596) H64(0.5272) H65(0.6341)
 H66(0.6732) H51A(0.5414) H51B(0.4918) H72(0.4799) H73(0.4071) H74(0.2947)
 H75(0.2531) H76(0.3236) H55A(0.4546) H55B(0.4269) H52A(0.5645) H52B(0.584)
 H82(0.6482) H83(0.7136) H84(0.8183) H85(0.8601) H86(0.7965) H53A(0.6697)
 H53B(0.589) H56A(0.7411) H56B(0.7023) H92(0.827) H93(0.8716) H94(0.8051)
 H95(0.6931) H96(0.6484) H54A(0.542) H54B(0.5973)
;
_shelx_res_checksum              53210
_shelx_hkl_checksum              37239
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'