Synthesis and Characterization of Magnesium and Aluminum Bis(phosphoranyl)methanediide Complexes
Guo, Jiayi; Lee, Jia-Shin; Foo, Ming-Choo; Lau, Kai-Chung; Xi, Hong-Wei; Lim, Kok Hwa; So, Cheuk-Wai; Organometallics 29 (2010) 939–; doi:10.1021/om900985f

data_4067502
_publ_section_title
;
 Synthesis and Characterization of Magnesium and Aluminum
 Bis(phosphoranyl)methanediide Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              939
_journal_paper_doi               10.1021/om900985f
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C58 H64 Al2 N2 P4 S2 Si2, 2(C4 H10 O)'
_chemical_formula_sum            'C66 H84 Al2 N2 O2 P4 S2 Si2'
_chemical_formula_weight         1235.49
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.99060(10)
_cell_length_b                   20.9657(3)
_cell_length_c                   15.5840(2)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.36
_cell_measurement_theta_min      2.18
_cell_volume                     3399.78(8)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69211
_diffrn_reflns_theta_full        33.84
_diffrn_reflns_theta_max         33.84
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.9217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         13555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                9782
_reflns_number_total             13555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900985f_si_001.cif
_cod_data_source_block           scw45s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3399.78(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4067502