Synthesis, Structures, and Reactions of Manganese Complexes Containing Diphosphine Ligands with Pendant Amines
Welch, Kevin D.; Dougherty, William G.; Kassel, W. Scott; DuBois, Daniel L.; Bullock, R. Morris; Organometallics 29 (2010) 4532–; doi:10.1021/om100668e

data_4066825
_publ_section_title
;
 Synthesis, Structures, and Reactions of Manganese Complexes Containing
 Diphosphine Ligands with Pendant Amines
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4532
_journal_paper_doi               10.1021/om100668e
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C88 H63.5 B F24.5 Mn N O P4'
_chemical_formula_weight         1806.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.6560(10)
_cell_angle_beta                 89.5880(10)
_cell_angle_gamma                80.3940(10)
_cell_formula_units_Z            4
_cell_length_a                   16.8661(7)
_cell_length_b                   22.7560(9)
_cell_length_c                   24.8001(10)
_cell_measurement_reflns_used    9716
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.86
_cell_volume                     8459.6(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.1180
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            149486
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.22
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.9274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3668
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Squeeze results consistent with one disordered solvent molecule of 
fluorobenzene per asymmetric unit.  The molecular formula has 
been adjusted to include this molecule.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2191
_refine_ls_number_reflns         64408
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                32348
_reflns_number_total             64408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100668e_si_002.cif
_cod_data_source_block           pnl035s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C176 H127 B2 F49 Mn2 N2 O2 P8'
_cod_original_formula_weight         3612.06
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066825