Reversible Cooperative Dihydrogen Binding and Transfer with a Bis-Phosphenium Complex of Chromium
Birchall, Nicholas; Feil, Christoph M.; Gediga, Michael; Nieger, Martin; Gudat, Dietrich; Chemical Science  (2020) –; doi:10.1039/D0SC03773G

data_1558895
_publ_section_title
;
 Reversible Cooperative Dihydrogen Binding and Transfer with a
 Bis-Phosphenium Complex of Chromium
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03773G
_journal_year                    2020
_chemical_formula_moiety         'C55 H73 Cr N4 O3 P2, C32 H12 B F24'
_chemical_formula_sum            'C87 H85 B Cr F24 N4 O3 P2'
_chemical_formula_weight         1815.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-26 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                95.414(1)
_cell_angle_beta                 99.551(1)
_cell_angle_gamma                92.236(1)
_cell_formula_units_Z            2
_cell_length_a                   12.5935(3)
_cell_length_b                   16.7577(4)
_cell_length_c                   21.3290(5)
_cell_measurement_reflns_used    11868
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      66.586
_cell_measurement_theta_min      2.111
_cell_volume                     4412.18(18)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65546
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        66.586
_diffrn_reflns_theta_max         66.586
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.291
_exptl_absorpt_correction_T_max  0.8690
_exptl_absorpt_correction_T_min  0.7319
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prism
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         15033
_refine_ls_number_restraints     2259
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0503P)^2^+2.7126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11868
_reflns_number_total             15033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03773g2.cif
_cod_data_source_block           g573_anis
_cod_database_code               1558895
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.808
_shelx_res_checksum              23505