Structures and CO2Reactivity of Zinc Complexes of Bis(diisopropyl-) and Bis(diphenylphosphino)amines
Dickie, Diane A.; Kemp, Richard A.; Organometallics 33 (2014) 6511–; doi:10.1021/om500856p

data_4084624
_publ_section_title
;
 Structures and CO2Reactivity of Zinc Complexes of Bis(diisopropyl-) and
 Bis(diphenylphosphino)amines
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6511
_journal_paper_doi               10.1021/om500856p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C48 H74 N2 O2 P4 Zn2'
_chemical_formula_weight         965.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.908(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2697(7)
_cell_length_b                   11.6675(5)
_cell_length_c                   22.8911(9)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      27.0585
_cell_measurement_theta_min      2.5317
_cell_volume                     4995.7(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker Direct Methods'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15207
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.201
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.585
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         10951
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+12.7876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                8560
_reflns_number_total             10951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500856p_si_001.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4084620--4084627.cif.'
_cod_database_code               4084624
_shelx_res_checksum              64594
_shelx_hkl_checksum              67701