Retrosynthetic approach to the design of molybdenum-magnesium oxoalkoxides.
Kuznetsov, Denis A.; Fedyanin, Ivan V.; Lyssenko, Konstantin A.; Bazhenova, Tamara A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12876–; doi:10.1039/c4dt01035c

data_7031417
_publ_section_title
;
 Retrosynthetic approach to the design of molybdenum-magnesium
 oxoalkoxides.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12876
_journal_paper_doi               10.1039/c4dt01035c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C68.6 H189.21 Mg6 Mo22 N12 O94'
_chemical_formula_weight         4942.78
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.464(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.983(2)
_cell_length_b                   24.133(3)
_cell_length_c                   21.952(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     8997(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL ver. 2009-9.1 (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL ver. 2009-9.1 (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega 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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75322
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, (Sheldrick, 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Solvate molecules located between the organometalic parts are disordered.
Although we were able to find separate partially occupied DMFA / Methanol
moieties they overlapped heavily with randomly distributed residual peaks.
We cannot exclude the presence in voids of dimethoxyethane molecules 
from the reaction mixture, as well as residual water addmixture. 
Therefore the whole part of the solvent was removed using the squeeze procedure
implemented in PLATON package (Spek 2009). We don't give exact moiety foumula,
because the real contents of the voids is unknown.
;
_refine_diff_density_max         1.946
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         19607
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1072P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                12030
_reflns_number_total             19607
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4dt01035c2.cif
_cod_data_source_block           momg_2_sq_rev2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031417--7031422.cif.
;
_cod_original_cell_volume        8996.7(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C68.60 H189.21 Mg6 Mo22 N12 O94'
_cod_database_code               7031417