Heterosynthon mediated tailored synthesis of pharmaceutical complexes: a solid-state NMR approach
Khan, Mujeeb; Enkelmann, Volker; Brunklaus, Gunther; CrystEngComm 13 (2011) 3213–; doi:10.1039/c0ce00657b

data_7205685
_publ_section_title
;
 Heterosynthon mediated tailored synthesis of pharmaceutical complexes:
 a solid-state NMR approach
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              3213
_journal_paper_doi               10.1039/c0ce00657b
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C27 H30 N2 O5'
_chemical_formula_sum            'C27 H30 N2 O5'
_chemical_formula_weight         462.55
_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
_audit_creation_date             09-09-23
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 92.126(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9147(5)
_cell_length_b                   36.1972(11)
_cell_length_c                   9.4766(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2370.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.078
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_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16522
_diffrn_reflns_theta_full        25.272
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         4.077
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         4813
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000233
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.61 1.97 0.627
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0816
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0806
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                4813
_reflns_number_total             5428
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            c0ce00657b.txt
_cod_data_source_block           khquin0909
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               7205685