Syntheses, structural characterisation and electronic structures of ferrocenyl-osmafuran heterobinuclear organometallic complexes
Liu, Bin; Guo, Chun-Lan; Liu, Wen-Xia; Guo, Ming-E.; Yan, Feng; Xue, Lu-Sha; Wang, Huijuan; Liu, Chang-Lin; Jin, Shan; Dalton Transactions  (2017) –; doi:10.1039/C7DT03145A

data_7044646
_publ_section_title
;
 Syntheses, structural characterisation and electronic structures of
 ferrocenyl-osmafuran heterobinuclear organometallic complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03145A
_journal_year                    2017
_chemical_formula_moiety
'C67 H55 Cl2 Fe O Os P3, 0.5(C8 H18), 2.56(C H2 Cl2)'
_chemical_formula_sum            'C73 H68 Cl6 Fe O Os P3'
_chemical_formula_weight         1512.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-24 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.2620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7133(10)
_cell_length_b                   20.3718(13)
_cell_length_c                   23.0817(15)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.79
_cell_measurement_theta_min      2.26
_cell_volume                     6733.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11780
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
N: Total Potential Solvent Accessible Void Vol ..................   513.6 Ang^3
N: Electron Count / Cell =    108 - To be included in D(calc), F000 & Mol.Wght.
Accoring to the analysis, the un-assigned disordered solvent molecues should 
be ca. 2.33 CH~2~Cl~2~ because it has been used in the crystallization of the
complex. Each host molecule can be distributed 0.56 CH~2~Cl~2~. Thus, the whole
formula is C~67~H~55~Cl~2~FeOOsP~3~, 0.5(C~8~H~18~), 2.56(CH~2~Cl~2~).
;
_refine_diff_density_max         2.820
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         11780
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+23.3188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                10260
_reflns_number_total             11780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03145a2.cif
_cod_data_source_block           mo_130626h_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7044646