Iron(II)/(NH)2P2Macrocycles: Modular, Highly Enantioselective Transfer Hydrogenation Catalysts
Bigler, Raphael; Huber, Raffael; Stöckli, Marco; Mezzetti, Antonio; ACS Catalysis 6 (2016) 6455–; doi:10.1021/acscatal.6b01872

data_4513940
_publ_section_title
;
 Iron(II)/(NH)2P2Macrocycles: Modular, Highly Enantioselective Transfer
 Hydrogenation Catalysts
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              6455
_journal_paper_doi               10.1021/acscatal.6b01872
_journal_volume                  6
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C57 H70 Fe N4 P2, 2(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C59 H74 B2 Cl4 F8 Fe N4 P2'
_chemical_formula_weight         1272.43
_chemical_name_common            '[Fe(CNAd)2(1b)](BF4)2, 2 CH2Cl2 (3c)'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                101.154(3)
_cell_angle_beta                 92.256(3)
_cell_angle_gamma                102.353(3)
_cell_formula_units_Z            1
_cell_length_a                   10.4939(10)
_cell_length_b                   10.7859(10)
_cell_length_c                   13.5065(13)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      37.105
_cell_measurement_theta_min      2.416
_cell_volume                     1459.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'Bruker SMART CCD 1K area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68309
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.159
_diffrn_reflns_theta_min         2.241
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.9373
_exptl_absorpt_correction_T_min  0.7974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1108 before and 0.0769 after correction.
The Ratio of minimum to maximum transmission is 0.8507.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.454
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 10272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.030(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         28919
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                24414
_reflns_number_total             28919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b01872_si_002.cif
_cod_data_source_block           new4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4513939--4513940.cif.
;
_cod_database_code               4513940
_shelxl_version_number           2013-4
_shelx_res_checksum              84954
_shelx_hkl_checksum              49606