High-Spin Manganese(II) Complexes of an Amido/Bis(Phosphine) PNP Ligand
Deborha Bacciu; Chun-Hsing Chen; Panida Surawatanawong; Bruce M. Foxman; Oleg V. Ozerov; Inorganic Chemistry 49 (2010) 5328–5334; doi:10.1021/ic1004424

data_4315678
_publ_section_title
;
 High-Spin Manganese(II) Complexes of an Amido/Bis(Phosphine) PNP Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5328
_journal_page_last               5334
_journal_paper_doi               10.1021/ic1004424
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C34 H56 Cl2 Li1 Mn1 N1 O2 P2'
_chemical_formula_sum            'C34 H56 Cl2 Li Mn N O2 P2'
_chemical_formula_weight         705.55
_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
_audit_creation_date             10-03-03
_audit_creation_method           CRYSTALS_ver_14.01
_cell_angle_alpha                90
_cell_angle_beta                 95.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1156(6)
_cell_length_b                   14.9784(8)
_cell_length_c                   25.7082(13)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     4261.9(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12604
_diffrn_reflns_theta_full        30.183
_diffrn_reflns_theta_max         30.183
_diffrn_reflns_theta_min         1.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.296
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there was disordered solvent (from 
history, likely pentane and/or THF) in a volume of 539.3 
\%A3 per unit cell (12.7%); the peaks could not be modeled 
successfully.  It appeared that the cavity areas contained 
about four pentane molecules, located near centers of 
symmetry at ( 1/2 1/2 0) and ( 1/2  0 1/2 ) as shown below.  
An initially satisfactory solution was obtained for the 
independent pentane molecule; however, residual peaks in 
the same area of 1.5 -- 2.0 e- suggested alternative 
partial occupancy of THF.  Modeling with or without 
restraints was unsuccessful, as was step by step 
acquisition of peaks using successive electron density 
difference maps.  Thus, the structure factors were 
modified using the PLATON SQUEEZE technique, in order 
to produce a ?solvate-free? structure factor set.  
PLATON reported a total electron density of 160 e- 
per unit cell, likely representing four pentane molecules 
(and/or substitution by THF), consistent with our earlier 
observations.  Use of the SQUEEZE technique resulted in a 
decrease of ca 1.3 % in R compared to unsatisfactory 
modeling.  
;
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9627
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         12604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.0110587
_refine_ls_shift/su_mean         2.4751880
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 3.49P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1394
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1394
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                9502
_reflns_number_total             12604
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      7.76
_oxford_refine_ls_r_factor_ref   0.0676
_oxford_refine_ls_scale          0.3400(3)
_oxford_reflns_number_all        12604
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ131_0m in P2(1)/c'
_cod_data_source_file            ic1004424_si_002_1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C34 H56 Cl2 Li1 Mn1 N1 O2 P2'
_cod_database_code               4315678