Stable Dihydrogen Complexes of Cobalt(-I) Suggest an Inverse trans-Influence of Lewis Acidic Group 13 Metalloligands.
Vollmer, Matthew V.; Xie, Jing; Lu, Connie C.; Journal of the American Chemical Society 139 (2017) 6570–6573; doi:10.1021/jacs.7b02870

data_4131280
_publ_section_title
;
 Stable Dihydrogen Complexes of Cobalt(-I) Suggest an Inverse
 trans-Influence of Lewis Acidic Group 13 Metalloligands.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6570
_journal_page_last               6573
_journal_paper_doi               10.1021/jacs.7b02870
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'2(C39 H60 Al Co N4 P3), C12 H29 Li O6, C12 H30 Li O6, C5 H12, C5 H11'
_chemical_formula_sum            'C112 H202 Al2 Co2 Li2 N8 O12 P6'
_chemical_formula_weight         2224.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.498(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3678(18)
_cell_length_b                   13.938(2)
_cell_length_c                   36.575(6)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.325
_cell_measurement_theta_min      4.447
_cell_volume                     6293.1(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  BrukerPhoton
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            136632
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.517
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   North1962
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       plate
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.060(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         31541
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+8.1355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.641
_reflns_Friedel_fraction_full    0.788
_reflns_Friedel_fraction_max     0.641
_reflns_number_gt                25885
_reflns_number_total             31543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02870_si_001.cif
_cod_data_source_block           mo_16285_0m
_cod_original_cell_volume        6293.1(17)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4131280
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              78172
_shelx_hkl_checksum              20875