Sodium, magnesium and zinc complexes of mono(phenolate) heteroscorpionate ligands
Schofield, A. Daniel; Barros, Mariana Luna; Cushion, Michael G.; Schwarz, Andrew D.; Mountford, Philip; Dalton Transactions  (2009) 85–96; doi:10.1039/b813116c

data_7000205
_publ_section_title
;
 Sodium, magnesium and zinc complexes of mono(phenolate)
 heteroscorpionate ligands
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              85
_journal_page_last               96
_journal_paper_doi               10.1039/b813116c
_journal_year                    2009
_chemical_formula_moiety         'C50 H70 Mg1 N8 O2 , C4 H10 O'
_chemical_formula_sum            'C54 H80 Mg N8 O3'
_chemical_formula_weight         913.59
_chemical_name_common            'Mg((Me2pz)2C(C6H2(tBu)2O)2 . OEt2'
_chemical_name_systematic
;
Mg{(Me2pz)2C(C6H2(tBu)2O}2 . OEt2
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.8818(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7496(4)
_cell_length_b                   17.6620(5)
_cell_length_c                   20.2696(5)
_cell_measurement_reflns_used    9336
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     5631.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17019
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_min         5.166
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1472
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.000396
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.34 0.676 0.973 -0.383E-01 0.150
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1249
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0879
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5266
_reflns_number_total             9832
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.81
_oxford_diffrn_Wilson_scale      28.40
_oxford_refine_ls_scale          0.2254(7)
_cod_data_source_file            b813116c.txt
_cod_data_source_block           compound_4.C4H10O
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C54 H80 Mg1 N8 O3'
_cod_database_code               7000205