Diastereoselective complex formation with a simple C2-symmetric hexadentate ligand based on a 1,1'-binaphthalene scaffold
Constable, Edwin C.; Zhang, Guoqi; Housecroft, Catherine E.; Neuburger, Markus; Schaffner, Silvia; Dalton Transactions  (2009) 8165–8167; doi:10.1039/b916996m

data_7002403
_publ_section_title
;
 Diastereoselective complex formation with a simple C2-symmetric
 hexadentate ligand based on a 1,1'-binaphthalene scaffold
;
_journal_coden_ASTM              DTARAF
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8165
_journal_page_last               8167
_journal_paper_doi               10.1039/b916996m
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         '(C42 H28 Fe N6), 2(B F4), 2(H2 O)'
_chemical_formula_sum            'C42 H32 B2 F8 Fe N6 O2'
_chemical_formula_weight         882.2
_space_group_IT_number           214
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I 41 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-01-05
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   30.4864(9)
_cell_length_b                   30.4864(9)
_cell_length_c                   30.4864(9)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    123
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     28334.7(14)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_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  0.064
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            80792
_diffrn_reflns_theta_full        26.390
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.889
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10704.337
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.76
_refine_diff_density_min         -1.00
_refine_ls_abs_structure_details 'Flack (1983), 2092 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     562
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.006688
_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:
0.584 0.530 0.241 -0.518E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1325
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0796
_reflns_limit_h_max              22
_reflns_limit_h_min              -20
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              2
_reflns_number_gt                3554
_reflns_number_total             4860
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.50
_oxford_diffrn_Wilson_scale      826.74
_oxford_refine_ls_r_factor_ref   0.0763
_oxford_refine_ls_scale          0.04582(15)
_oxford_reflns_number_all        4824
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'gq46_123k_0m in I-43m'
_cod_data_source_file            B916996M.txt
_cod_data_source_block           gq46_123k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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      'I 41 3 2 '
_cod_original_formula_sum        'C42 H32 B2.00 F8.00 Fe1 N6 O2.00'
_cod_database_code               7002403