Hydroxyethylmethacrylate as a source of ethyleneglycolate ligands. Synthesis and characterization of Nb4(μ,η1,η2-OC2H4O)2(μ3,η1,η2-OC2H4O)2(μ-OC2H4O)(OPri)10
Hubert-Pfalzgraf, Liliane G.; Abada, Valérie; Vaissermann, Jacqueline; Journal of the Chemical Society, Dalton Transactions  (1999) 2407–; doi:10.1039/a904344f

data_7027582
_publ_contact_author
;
 Pr L. G. Hubert-Pfalzgraf                         
;
_publ_section_title
;
 Hydroxyethylmethacrylate as a source of ethyleneglycolate ligands.
 Synthesis and characterization of
 Nb4(\m,\h1,\h2-OC2H4O)2(\m3,\h1,\h2-OC2H4O)2(\m-OC2H4O)(OPri)10
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2407
_journal_paper_doi               10.1039/a904344f
_journal_year                    1999
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C40 H90 Nb4 O20 '
_chemical_formula_sum            'C40 H90 Nb4 O20'
_chemical_formula_weight         1262.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-04-09
_audit_creation_method           CRYSTALS
_cell_angle_alpha                78.86(3)
_cell_angle_beta                 74.24(3)
_cell_angle_gamma                78.84(2)
_cell_formula_units_Z            2
_cell_length_a                   17.938(5)
_cell_length_b                   17.960(5)
_cell_length_c                   9.335(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    161
_cell_volume                     2808.0(19)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      161
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  ' graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3433
_diffrn_reflns_theta_max         17
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        6.56
_diffrn_standards_interval_time  3600s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.82
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            '  '
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_description       '  '
_exptl_crystal_F_000             1290.48
_refine_diff_density_max         1.95
_refine_diff_density_min         -0.82
_refine_ls_extinction_coef       none
_refine_ls_goodness_of_fit_obs   1.1257
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle,
 one overall isotropic thermal parameter refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         2703
_refine_ls_R_factor_obs          0.0692
_refine_ls_shift/esd_max         1.086399
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0801
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_observed          2703
_reflns_number_total             3267
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            904344fsup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '161K' was changed to '161' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '161K' was changed
to '161' - the value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value ' triclinic ' changed to
'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_matrix_type' value ' full' changed to 'full'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value ' Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value ' Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2807(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C40 H90 Nb4 O20 '
_cod_database_code               7027582