Matrixes in UV-MALDI mass spectrometry ‒ crystals of organic salts versus co-crystals of neutral polyfunctional carboxylic acids
Ivanova, Bojidarka B.; Analytical Methods 4 (2012) 2247–; doi:10.1039/c2ay25090j

data_1514929
_publ_section_title
;
 Matrixes in UV-MALDI mass spectrometry -- crystals of organic salts
 versus co-crystals of neutral polyfunctional carboxylic acids
;
_journal_issue                   8
_journal_name_full               'Analytical Methods'
_journal_page_first              2247
_journal_paper_doi               10.1039/c2ay25090j
_journal_volume                  4
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C8 H19 N2 O2, C8 H8 O3, C8 H7 O3'
_chemical_formula_sum            'C24 H34 Cl0 N2 O8'
_chemical_formula_weight         478.53
_chemical_melting_point          344
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.711(3)
_cell_length_b                   12.974(6)
_cell_length_c                   23.865(11)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    199(2)
_cell_measurement_theta_max      19.21
_cell_measurement_theta_min      2.32
_cell_volume                     2387.5(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker GIS'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      199(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.18
_diffrn_reflns_av_sigmaI/netI    0.1904
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12494
_diffrn_reflns_theta_full        19.21
_diffrn_reflns_theta_max         19.21
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9922
_exptl_absorpt_correction_T_min  0.9880
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(5)
_refine_ls_extinction_coef       0.000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         1935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.1047
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2338
_reflns_number_gt                1484
_reflns_number_total             1935
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             1513044
_cod_data_source_file            c2ay25090j.txt
_cod_data_source_block           200-10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '344K' was changed to '344' - the
value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 

 Removing Professor Michael Spiteller's name from the authors' list as
 requested in the addendum
 http://www.rsc.org/suppdata/ay/c2/c2ay25090j/addition.htm

 Saulius Gra\<zulis
 2014-10-05

;
_cod_original_cell_volume        2387.3(19)
_cod_database_code               1514929