Structural Diversity in Alkali Metal Complexes of Sterically Demanding Carbazol-9-yl Ligands
Rhiannon S. Moorhouse; Graeme J. Moxey; Fabrizio Ortu; Thomas J. Reade; William Lewis; Alexander J. Blake; Deborah L. Kays; Inorganic Chemistry 52 (2013) 2678–2683; doi:10.1021/ic302727w

data_4334052
_publ_contact_author_address
;  School of Chemistry, University of Nottingham,
   University Park,
   Nottingham, NG7 2RD, United Kingdom
;
_publ_contact_author_email       Deborah.Kays@nottingham.ac.uk
_publ_contact_author_fax         '+44-(0) 115 951 3461'
_publ_contact_author_name        'Deborah L. Kays'
_publ_contact_author_phone       '+49-(0) 115 951 3555'
_publ_section_title
;
 Structural Diversity in Alkali Metal Complexes of Sterically Demanding
 Carbazol-9-yl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2678
_journal_page_last               2683
_journal_paper_doi               10.1021/ic302727w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C40 H64 N Na O3'
_chemical_formula_sum            'C40 H64 N Na O3'
_chemical_formula_weight         629.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.524(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.997(3)
_cell_length_b                   17.624(3)
_cell_length_c                   16.003(3)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.26
_cell_volume                     3803.7(13)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.102
_diffrn_reflns_av_sigmaI/netI    0.149
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23212
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.29
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.182
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.092P)^2^+1.043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.188
_refine_ls_wR_factor_ref         0.226
_reflns_number_gt                4381
_reflns_number_total             8731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302727w_si_001_4.cif
_cod_data_source_block           2.3THF
_cod_original_cell_volume        3803.7(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4334052