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_7035161
_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         'C37 H51 Mn N8 O, C F3 O3 S, C4 H8 O'
_chemical_formula_sum            'C42 H60 F3 Mn N8 O5 S'
_chemical_formula_weight         827.48
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-16 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0279(13)
_cell_length_b                   23.222(2)
_cell_length_c                   26.969(2)
_cell_measurement_reflns_used    5004
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      52.87
_cell_measurement_theta_min      3.28
_cell_volume                     9411.6(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_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 0.984
_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  cc66das-sr
_diffrn_reflns_av_R_equivalents  0.1370
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            8372
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.324
_diffrn_reflns_theta_min         3.277
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  0.8102
_exptl_absorpt_correction_T_min  0.2452
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3478
_exptl_crystal_id                cc66das-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 (3, -1, 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.722
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.104
_platon_squeeze_details
; 
There were a total of 101 electrons squeezed out per asymmetric 
unit.  This corresponds to 2.5 tetrahydrofuran molecules in each asymmetric 
unit. 
;
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         8372
_refine_ls_number_restraints     1691
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+4.3486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6071
_reflns_number_total             8372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00985e2.cif
_cod_data_source_block           cc66das-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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.

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

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035158--7035164.cif.
;
_cod_original_cell_volume        9411.6(14)
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               7035161
_shelx_estimated_absorpt_t_min   0.209
_shelx_estimated_absorpt_t_max   0.735
_shelxl_version_number           2014-3
_shelx_res_checksum              46892