Solid State Structures and Dynamic Solution Equilibria of Bis(dibenzylamido)magnesium Complexes: Aggregation Dependence on Stoichiometry and Denticity of Donor Solvent
William Clegg; Fiona J. Craig; Kenneth W. Henderson; Alan R. Kennedy; Robert E. Mulvey; Paul A. O'Neil; David Reed; Inorganic Chemistry 36 (1997) 6238–6246; doi:10.1021/ic970912a

data_4323763
_publ_section_title
;
 Solid State Structures and Dynamic Solution Equilibria of
 Bis(dibenzylamido)magnesium Complexes: Aggregation Dependence on
 Stoichiometry and Denticity of Donor Solvent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6238
_journal_page_last               6246
_journal_paper_doi               10.1021/ic970912a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C71.5 H98 Mg2 N10 O2 P2'
_chemical_formula_weight         1240.16
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.588(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   14.7440(6)
_cell_length_b                   21.4484(8)
_cell_length_c                   66.996(3)
_cell_measurement_reflns_used    61125
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      1.81
_cell_volume                     21178.4(15)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            88160
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             8004
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2381
_refine_ls_number_reflns         29456
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_obs          0.0647
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+33.3881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1533
_refine_ls_wR_factor_obs         0.1429
_reflns_number_observed          23485
_reflns_number_total             29456
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970912a_3.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+33.3881P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+33.3881P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C71.50 H98 Mg2 N10 O2 P2'
_cod_database_code               4323763