The first stereoselective syntheses of 2,2'-biindoline
Steven Wales; Anthony Willis; Paul Keller; Chem.Commun. 46 (2010) 9226–; doi:10.1039/c0cc04045b

data_7105737
_publ_section_title
;
 The first stereoselective syntheses of 2,2'-biindoline
;
_journal_name_full               Chem.Commun.
_journal_page_first              9226
_journal_paper_doi               10.1039/c0cc04045b
_journal_volume                  46
_journal_year                    2010
_chemical_absolute_configuration rmad
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_moiety         'C16 H16 Cl2 N2 Pd, 0.225(C2 H3 N)'
_chemical_formula_sum            'C16.45 H16.675 Cl2 N2.225 Pd'
_chemical_formula_weight         422.86
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-05-25
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-05-22 - Report on C16.44 H16.66 Cl2 N2.22 Pd1
by Anthony C. Willis
for Paul Keller

2009-05-22 - passes checkcif tests with minor warnings
2009-05-25 - new version to fix poor C-H bonds
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0215(6)
_cell_length_b                   8.2900(2)
_cell_length_c                   9.0928(3)
_cell_measurement_reflns_used    21993
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1584.59(8)
_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
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_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  0.038
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14560
_diffrn_reflns_theta_full        27.469
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         2.641
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             841.073
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.40
_refine_ls_abs_structure_details 'Flack (1983), 1531 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8545
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3618
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.028927
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0507
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0507
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                3235
_reflns_number_total             3618
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.30
_oxford_diffrn_Wilson_scale      6.22
_oxford_refine_ls_r_factor_ref   0.0267
_oxford_refine_ls_scale          0.4035(3)
_oxford_reflns_number_all        3618
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'transf axes for std setting of sp gp'
_cod_data_source_file            C0CC04045B.TXT
_cod_data_source_block           wol0903
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_original_formula_sum        'C16.450 H16.675 Cl2 N2.225 Pd1'
_cod_database_code               7105737