Synthesis and reactivity of TADDOL-based chiral Fe(ii) PNP pincer complexes-solution equilibria between κ(2)P,N- and κ(3)P,N,P-bound PNP pincer ligands.
Holzhacker, Christian; Stöger, Berthold; Carvalho, Maria Deus; Ferreira, Liliana P.; Pittenauer, Ernst; Allmaier, Günter; Veiros, Luis F.; Realista, Sara; Gil, Adrià; Calhorda, Maria José; Müller, Danny; Kirchner, Karl; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13071–13086; doi:10.1039/c5dt00832h

data_7035416
_publ_section_title
;
 Synthesis and reactivity of TADDOL-based chiral Fe(ii) PNP pincer
 complexes-solution equilibria between \k(2)P,N- and \k(3)P,N,P-bound PNP
 pincer ligands.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13071
_journal_page_last               13086
_journal_paper_doi               10.1039/c5dt00832h
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C46 H55 Br2 Fe N3 O5 P2'
_chemical_formula_weight         1007.6
_chemical_name_systematic        ' ?'
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_update_record
;
2014-11-05 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                93.0205(19)
_cell_angle_beta                 93.3464(18)
_cell_angle_gamma                91.2982(19)
_cell_formula_units_Z            2
_cell_length_a                   9.1105(5)
_cell_length_b                   10.3931(6)
_cell_length_c                   24.1374(14)
_cell_measurement_reflns_used    9120
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.3
_cell_volume                     2277.7(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2014)'
_computing_molecular_graphics    Mercury
_computing_structure_refinement
'Jana2006 (Pet\<r\'i\<cek <i>et al.</i>, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55010
_diffrn_reflns_theta_full        30.2
_diffrn_reflns_theta_max         30.2
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.4691
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
'  12513 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.011(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    0.93
_refine_ls_goodness_of_fit_ref   0.87
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    443
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         25848
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0293
_refine_ls_shift/su_mean         0.0019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0379
_reflns_number_gt                19167
_reflns_number_total             25848
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c5dt00832h2.cif
_cod_data_source_block           Fe_PNP_TAD_iPr_Br2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035416--7035418.cif.
;
_cod_original_formula_sum        'C46 H55 Br2 Fe1 N3 O5 P2'
_cod_database_code               7035416