The isolation of a metastable conglomerate using a combined computational and controlled crystallization approach
Roger J. Davey; Ghazala Sadiq; Kevin Back; Laura Wilkinson; Colin C. Seaton; Chem.Commun. 48 (2012) 1976–; doi:10.1039/c1cc16173c

data_7107329
_publ_section_title
;
 The isolation of a metastable conglomerate using a combined computational
 and controlled crystallization approach
;
_journal_name_full               Chem.Commun.
_journal_page_first              1976
_journal_paper_doi               10.1039/c1cc16173c
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C8 H7 Cl O3'
_chemical_formula_sum            'C8 H7 Cl O3'
_chemical_formula_weight         186.59
_chemical_name_common            '(S)-2-chloromandelic acid'
_chemical_name_systematic
;
S-(2-chlorophenyl)(hydroxy)acetic acid
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.997(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0612(4)
_cell_length_b                   7.4986(3)
_cell_length_c                   13.8910(6)
_cell_measurement_reflns_used    2933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4391
_cell_measurement_theta_min      3.1069
_cell_volume                     807.16(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
1 omega -107.00 78.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -21.2308 0.0000 -60.0000 185

2 omega -86.00 -29.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -21.2308 137.0000 -87.0000 57

3 omega -84.00 -58.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -21.2308 179.0000 150.0000 26

4 omega -6.00 40.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.6371 -77.0000 60.0000 46

5 omega 22.00 83.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.6371 -131.0000 -154.0000 61
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0612108801
_diffrn_orient_matrix_UB_12      -0.0256914653
_diffrn_orient_matrix_UB_13      0.0255450219
_diffrn_orient_matrix_UB_21      0.0631092126
_diffrn_orient_matrix_UB_22      0.0122006106
_diffrn_orient_matrix_UB_23      0.0466274257
_diffrn_orient_matrix_UB_31      -0.0259613667
_diffrn_orient_matrix_UB_32      0.0902280074
_diffrn_orient_matrix_UB_33      0.0009681230
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5399
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3003
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                2596
_reflns_number_total             3003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16173c.txt
_cod_data_source_block           2CLMA
_cod_original_cell_volume        807.16(6)
_cod_database_code               7107329