Cooperative H2 Activation across a Metal‒Metal Multiple Bond and Hydrogenation Reactions Catalyzed by a Zr/Co Heterobimetallic Complex
Gramigna, Kathryn M.; Dickie, Diane A.; Foxman, Bruce M.; Thomas, Christine M.; ACS Catalysis 9 (2019) 3153–; doi:10.1021/acscatal.8b04390

data_4514744
_publ_section_title
;
 Cooperative H2 Activation across a Metal--Metal Multiple Bond and
 Hydrogenation Reactions Catalyzed by a Zr/Co Heterobimetallic Complex
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              3153
_journal_paper_doi               10.1021/acscatal.8b04390
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C45 H69 Co I N2 O P3 Zr'
_chemical_formula_sum            'C45 H69 Co I N2 O P3 Zr'
_chemical_formula_weight         1023.98
_chemical_name_systematic        C45H69CoIN2OP3Zr
_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     dual
_audit_creation_date             2018-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                70.756(2)
_cell_angle_beta                 71.300(2)
_cell_angle_gamma                74.862(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2182(7)
_cell_length_b                   13.3740(7)
_cell_length_c                   16.9003(9)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      32.573
_cell_measurement_theta_min      2.931
_cell_volume                     2432.1(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            141522
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.686
_diffrn_reflns_theta_min         2.948
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0810 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.8395.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_recrystallization_method
'Crystallized from pentane at room temperature'
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         17767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+3.9187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14930
_reflns_number_total             17767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04390_si_002.cif
_cod_data_source_block           4-PMePh2
_cod_database_code               4514744
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H45C)=Sof(H45D)=Sof(H42C)=Sof(H42D)=Sof(C43)=Sof(H43C)=Sof(H43D)=
 Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(H45A)=Sof(H45B)=Sof(H42A)=Sof(H42B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C43A)=Sof(H43A)=Sof(H43B)=FVAR(1)
 Sof(C36A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=
 Sof(C38A)=Sof(H38A)=Sof(C37A)=Sof(H37A)=1-FVAR(2)
 Sof(C36)=Sof(C41)=Sof(H41)=Sof(C37)=Sof(H37)=Sof(C40)=Sof(H40)=Sof(C38)=
 Sof(H38)=Sof(C39)=Sof(H39)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C26(H26), C9(H9), C23(H23)
3.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C45(H45C,H45D), C42(H42A,H42B), C42(H42C,H42D), C44(H44A,
 H44B), C43A(H43A,H43B), C43(H43C,H43D), C44A(H44C,H44D)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C20(H20), C6(H6), C31(H31), C2(H2), C35(H35), C18(H18), C33(H33),
 C4(H4), C34(H34), C32(H32), C41(H41), C37(H37), C40(H40), C38(H38), C39(H39),
 C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A), C37A(H37A)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C13(H13A,H13B,H13C), C11(H11A,H11B,
 H11C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C25(H25A,
 H25B,H25C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C),
 C27(H27A,H27B,H27C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              57910
_shelx_hkl_checksum              28019
_olex2_exptl_crystal_mounting_method
'A red plate-like specimen of C45H69CoIN2OP3Zr was coated with Paratone oil and mounted on a MiTeGen MicroLoop that had been previously attached to a metallic pin using epoxy for the X-ray crystallographic analysis.'
_olex2_submission_original_sample_id C45H69CoIN2OP3Zr
_olex2_submission_special_instructions 'No special instructions were received'