π-Stacking and hydrogen bonding direct diastereoselectivity in one-pot syntheses of octahedral iron(ii) complexes
Constable, Edwin C.; Zhang, Guoqi; Housecroft, Catherine E.; Neuburger, Markus; Zampese, Jennifer A.; Chemical Communications 46 (2010) 3077–3079; doi:10.1039/b927071j

data_7105500
_publ_section_title
;
 \p-Stacking and hydrogen bonding direct diastereoselectivity in
 one-pot syntheses of octahedral iron(ii) complexes
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              3077
_journal_page_last               3079
_journal_paper_doi               10.1039/b927071j
_journal_volume                  46
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
C38 H28 Fe N6 O2, 2(F6 P), 0.339(C2 H6 O), 0.219(H2 O)
;
_chemical_formula_sum            'C38.68 H34.47 F12 Fe N6 O2.56 P2'
_chemical_formula_weight         970.10
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-02-03
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 116.081(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.077(2)
_cell_length_b                   10.3578(10)
_cell_length_c                   18.6921(16)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    123
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     4186.9(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa Apex2'
_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  0.027
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58777
_diffrn_reflns_theta_full        30.275
_diffrn_reflns_theta_max         30.893
_diffrn_reflns_theta_min         1.735
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1962.114
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.87
_refine_diff_density_min         -1.47
_refine_ls_abs_structure_details 'Flack (1983), 6231 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.018(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1068
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9916
_refine_ls_number_restraints     1069
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.008210
_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:
0.422 0.442 0.139
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0969
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0746
_reflns_limit_h_max              31
_reflns_limit_h_min              -34
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11426
_reflns_number_total             13132
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.40
_oxford_diffrn_Wilson_scale      309.39
_oxford_refine_ls_r_factor_ref   0.0653
_oxford_refine_ls_scale          0.07682(14)
_oxford_reflns_number_all        13098
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'gq111_2_123k_0m in C2'
_cod_data_source_file            B927071J.txt
_cod_data_source_block           2
_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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4186.8(7)
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C38.68 H34.47 F12 Fe1 N6 O2.56 P2'
_cod_database_code               7105500