Exploiting Synthetic Conditions to Promote Structural Diversity within the Scandium(III)/Pyrimidine-4,6-dicarboxylate System
Cepeda, Javier; Pérez-Yáñez, Sonia; Beobide, Garikoitz; Castillo, Oscar; Luque, Antonio; Wright, Paul A.; Sneddon, Scott; Ashbrook, Sharon E.; Crystal Growth & Design 15 (2015) 2352–; doi:10.1021/acs.cgd.5b00154

data_4513068
_publ_contact_author
;
Javier Cepeda. Departamento de Quimica Inorganica. 
Facultad de Ciencia y Tecnologia
Universidad del Pais Vasco,  Apdo. 644, 
E-48080 Bilbao, Spain
;
_publ_section_title
;
 Exploiting Synthetic Conditions to Promote Structural Diversity within
 the Scandium(III)/Pyrimidine-4,6-dicarboxylate System
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2352
_journal_paper_doi               10.1021/acs.cgd.5b00154
_journal_volume                  15
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C4 O8 Sc, (NH4)'
_chemical_formula_structural     'C4 O8 Sc, (NH4)'
_chemical_formula_sum            'C4 H4 N O8 Sc'
_chemical_formula_weight         239.09
_chemical_name_systematic
;
 Poly{ammonium[bis(mu-oxalato-k2O,O':k2O'',O''')scandate(III)]}
;
_space_group_IT_number           180
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      180
_symmetry_space_group_name_Hall  'P 62 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 62 2 2'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   8.5940(8)
_cell_length_b                   8.5940(8)
_cell_length_c                   12.4441(5)
_cell_measurement_reflns_used    5772
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.74
_cell_volume                     795.95(11)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5572
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.992
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.1106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1765P)^2^+9.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3226
_refine_ls_wR_factor_ref         0.3258
_reflns_number_gt                546
_reflns_number_total             587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00154_si_002.cif
_cod_data_source_block           Compound3
_cod_original_cell_volume        795.95(9)
_cod_original_sg_symbol_Hall     'P 62 2 (004)'
_cod_database_code               4513068