Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis of H2
Stolley, Ryan M.; Darmon, Jonathan M.; Das, Parthapratim; Helm, Monte L.; Organometallics 35 (2016) 2965–; doi:10.1021/acs.organomet.6b00486

data_4088846
_publ_section_title
;
 Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis
 of H2
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2965
_journal_paper_doi               10.1021/acs.organomet.6b00486
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C30 H43 N P2'
_chemical_formula_sum            'C30 H43 N P2'
_chemical_formula_weight         479.63
_chemical_name_systematic
meso-1-benzhydryl-3,7-dicyclohexyl-1,3,7-azadiphosphocane
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-27
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.034(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.6899(3)
_cell_length_b                   25.6850(12)
_cell_length_c                   9.5148(4)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.375
_cell_volume                     1329.54(11)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34591
_diffrn_reflns_theta_full        28.7480
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0527 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9308.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1980
_exptl_crystal_description       plate
_exptl_crystal_F_000             520.5730
_exptl_crystal_preparation       'isothermal evaporation of toluene solution'
_exptl_crystal_recrystallization_method
'isothermal evaporation of toluene solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.9892
_refine_diff_density_min         -0.2886
_refine_diff_density_rms         0.0622
_refine_ls_d_res_high            0.7389
_refine_ls_d_res_low             12.8425
_refine_ls_goodness_of_fit_ref   1.0558
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0558
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.8835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3177
_reflns_number_total             3515
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om6b00486_si_002.cif
_cod_data_source_block           stol017_0m
_cod_database_code               4088846
_olex2_refinement_description
;
1. Others
 Fixed U12: N2(0) C4(0) C1(0)
 Fixed U23: N2(0) C4(0) C1(0)
 Fixed Y: N2(0.75) C4(0.75) H4(0.75) C1(0.75) H1a(0.75) H1b(0.75)
;