1,2-Addition of Formic or Oxalic Acid to‒N{CH2CH2(PiPr2)}2-Supported Mn(I) Dicarbonyl Complexes and the Manganese-Mediated Decomposition of Formic Acid
Tondreau, Aaron M.; Boncella, James M.; Organometallics 35 (2016) 2049–; doi:10.1021/acs.organomet.6b00274

data_4086573
_publ_section_title
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 1,2-Addition of Formic or Oxalic Acid to--N{CH2CH2(PiPr2)}2-Supported
 Mn(I) Dicarbonyl Complexes and the Manganese-Mediated Decomposition of
 Formic Acid
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_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2049
_journal_paper_doi               10.1021/acs.organomet.6b00274
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C18 H36 Mn N O2 P2'
_chemical_formula_weight         415.38
_chemical_name_systematic
; 
 ? 
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.7910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.2679(9)
_cell_length_b                   22.5860(14)
_cell_length_c                   14.7260(9)
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.30
_cell_volume                     4285.7(5)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80634
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.7591
_exptl_absorpt_correction_T_min  0.7180
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0073(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         14252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0438P)^2^+1.5347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                11344
_reflns_number_total             14252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00274_si_002.cif
_cod_data_source_block           iprpnhpmnco2
_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 'Empirical' changed to
'empirical' 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 4624 2016-04-14 12:54:50Z antanas 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4086573