Synthesis and characterization of M(ii) (M = Mn, Fe and Co) azafulvene complexes and their X3(-) derivatives.
Matson, Ellen M.; Park, Yun Ji; Bertke, Jeffery A.; Fout, Alison R.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10377–10384; doi:10.1039/c5dt00985e

data_7035160
_publ_section_title
;
 Synthesis and characterization of M(ii) (M = Mn, Fe and Co) azafulvene
 complexes and their X3(-) derivatives.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10377
_journal_page_last               10384
_journal_paper_doi               10.1039/c5dt00985e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'2(C37 H51 Mn N8 S), 2(C F3 O3 S), 1.5(C6 H6)'
_chemical_formula_sum            'C85 H111 F6 Mn2 N16 O6 S4'
_chemical_formula_weight         1805.02
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-16 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6420(3)
_cell_length_b                   23.5381(5)
_cell_length_c                   25.1862(6)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      67.59
_cell_measurement_theta_min      2.60
_cell_volume                     9075.6(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  cc72dsa-sr
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            61703
_diffrn_reflns_theta_full        68.12
_diffrn_reflns_theta_max         68.12
_diffrn_reflns_theta_min         2.60
_diffrn_standards_number         16070
_exptl_absorpt_coefficient_mu    3.719
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.7845
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3796
_exptl_crystal_id                cc72dsa-sr
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) 
with the (0, -1, -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.208
_platon_squeeze_details
; 
There were a total of 34 electrons squeezed out per asymmetric 
unit.  This corresponds to a single diethylether molecule in each asymmetric 
unit. 
;
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         16070
_refine_ls_number_restraints     307
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.9429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                13635
_reflns_number_total             16070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00985e2.cif
_cod_data_source_block           cc72das-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 7035158--7035164.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7035160