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_7030516
_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(F6 P)'
_chemical_formula_sum            'C42 H28 F12 Fe N6 P2'
_chemical_formula_weight         962.50
_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             09-02-19
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8971(6)
_cell_length_b                   19.2376(7)
_cell_length_c                   10.9316(4)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    123
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3763.7(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.037
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            93115
_diffrn_reflns_theta_full        30.544
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.863
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.57
_refine_ls_abs_structure_details 'Flack (1983), 5165 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.006(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2586
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.006319
_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:
0.132 0.877E-01 0.313E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0503
_refine_ls_wR_factor_gt          0.0349
_refine_ls_wR_factor_ref         0.0333
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                10004
_reflns_number_total             11517
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.42
_oxford_diffrn_Wilson_scale      120.16
_oxford_refine_ls_r_factor_ref   0.0304
_oxford_refine_ls_scale          0.08788(7)
_oxford_reflns_number_all        11487
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'gq55_123k_0ma in P2(1)2(1)2'
_cod_duplicate_entry             7002404
_cod_data_source_file            b916996m.txt
_cod_data_source_block           gq55_123k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 
;
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_original_formula_sum        'C42 H28 F12 Fe1 N6 P2'
_cod_database_code               7030516