Formation of a Reversible, Intramolecular Main-Group Metal-CO2 Adduct
Diane A. Dickie; Eric N. Coker; Richard A. Kemp; Inorganic Chemistry 50 (2011) 11288–11290; doi:10.1021/ic201697g

data_4326903
_publ_section_title
;
 Formation of a Reversible, Intramolecular Main-Group Metal-CO2 Adduct
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11288
_journal_page_last               11290
_journal_paper_doi               10.1021/ic201697g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C12 H29 N P2'
_chemical_formula_weight         249.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.590(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.0394(14)
_cell_length_b                   8.7728(4)
_cell_length_c                   9.9798(4)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.59
_cell_volume                     3127.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            58695
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.8962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.941
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         8400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+24.3554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2600
_refine_ls_wR_factor_ref         0.2627
_reflns_number_gt                7488
_reflns_number_total             8400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201697g_si_001.cif
_cod_data_source_block           rkdd112a
_cod_database_code               4326903