Synthesis, coordination behavior and structural features of chiral iron(II) PNP diferrocene complexes
Zirakzadeh, Afrooz -; Karl, Kirchner; Roller, Alexander; Stöger, Berthold; Carvalho, Maria de Deus; Ferreira, Liliana; RSC Adv.  (2016) –; doi:10.1039/C5RA26493F

data_7223953
_publ_section_title
;
 Synthesis, coordination behavior and structural features of chiral
 iron(II) PNP diferrocene complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA26493F
_journal_year                    2016
_chemical_formula_moiety         'C46 H39 Br2 Fe3 N P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H43 Br2 Cl4 Fe3 N P2'
_chemical_formula_weight         1164.94
_chemical_name_common            (SFc,SFc)-11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-05 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3358(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3149(3)
_cell_length_b                   18.7337(7)
_cell_length_c                   13.9965(5)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.114
_cell_measurement_theta_min      2.458
_cell_volume                     2422.43(15)
_computing_cell_refinement       'APEX2 v2013.6-0'
_computing_data_collection       'APEX2 v2013.6-0'
_computing_data_reduction        'APEX2 v2013.6-0'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54673
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.116
_diffrn_reflns_theta_min         2.174
_diffrn_source                   'INCOATEC microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0705 before and 0.0391 after correction. 
The Ratio of minimum to maximum transmission is 0.8587. 
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 6361 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0114(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         14257
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+2.4270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.942
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                13656
_reflns_number_total             14257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26493f2.cif
_cod_data_source_block           afzi814_P21
_cod_database_code               7223953
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              47961