Attempted Syntheses of Transition Metal and Lanthanide (Dialkylamino)squarates. The Hydrolysis Problem
Hazel-Ann Hosein; Lincoln A. Hall; Alan J. Lough; William Desmarais; Michael J. Vela; Bruce M. Foxman; Inorganic Chemistry 37 (1998) 4184–4189; doi:10.1021/ic9801490

data_4322956
_publ_contact_author
;
Bruce M. Foxman
Department of Chemistry
Brandeis University - MS 015
Waltham, MA 02254-9110 USA
;
_publ_contact_author_email       ' foxman1@binah.cc.brandeis.edu  '
_publ_contact_author_fax         ' 1 617 736 2516 '
_publ_contact_author_phone       ' 1 617 736 2532 '
_publ_section_title
;
 Attempted Syntheses of Transition Metal and Lanthanide
 (Dialkylamino)squarates. The Hydrolysis Problem
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4184
_journal_page_last               4189
_journal_paper_doi               10.1021/ic9801490
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C6 H7 O3 N1 '
_chemical_formula_sum            'C6 H7 N O3'
_chemical_formula_weight         141.13
_chemical_name_systematic        1-(dimethylamino)-2-hydroxycyclobutenedione
_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
_audit_creation_date             97-12-18
_audit_creation_method           CRYSTALS_ver_07-07-97
_cell_angle_alpha                90.
_cell_angle_beta                 95.121(12)
_cell_angle_gamma                90.
_cell_formula_units_Z            4.00
_cell_length_a                   5.0933(7)
_cell_length_b                   8.3314(6)
_cell_length_c                   15.087(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      46
_cell_measurement_theta_min      41
_cell_volume                     637.65(16)
_computing_cell_refinement       'CAD4-EXPRESS (Straver, 1992)'
_computing_data_collection       'CAD4-EXPRESS (Straver, 1992)'
_computing_data_reduction
;
MolEN (Fair, C. K., 1990)
;
_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)
;
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1350
_diffrn_reflns_theta_max         74.30
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  7200s
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.98
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.47
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' cube '
_exptl_crystal_F_000             297.04
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.25
_refine_ls_extinction_coef       29.3(26)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0364
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1157
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/su_max          0.107539
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Chebychev polynomial with   3 parameters (Carruthers & Watkin, 1979)
 2.65 1.54 1.62
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0425
_reflns_limit_h_max              6
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_observed          1157
_reflns_number_total             1299
_reflns_observed_criterion       >1.96\s(I)
_cod_data_source_file            ic9801490.cif
_cod_data_source_block           IC9801490-Structure_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

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        637.66
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C6 H7 O3 N1 '
_cod_database_code               4322956