Synthesis and Structure of Allyl and Alkynyl Complexes of Manganese(II) Supported by a Bulky β-Diketiminate Ligand
Chai, Jianfang; Zhu, Hongping; Roesky, Herbert W.; Yang, Zhi; Jancik, Vojtech; Herbst-Irmer, Regine; Schmidt, Hans-Georg; Noltemeyer, Mathias; Organometallics 23 (2004) 5003–5006; doi:10.1021/om049605k

data_4087352
_publ_section_title
;
 Synthesis and Structure of Allyl and Alkynyl Complexes of Manganese(II)
 Supported by a Bulky \b-Diketiminate Ligand
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5003
_journal_page_last               5006
_journal_paper_doi               10.1021/om049605k
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C37 H46 Mn N2'
_chemical_formula_weight         573.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 98.59(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.010(1)
_cell_length_b                   13.257(1)
_cell_length_c                   17.697(1)
_cell_measurement_reflns_used    4637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.95
_cell_measurement_theta_min      3.75
_cell_volume                     3250.0(4)
_computing_cell_refinement       'Siemens SAINT (V. 6.31a, Siemens 2002)'
_computing_data_collection       'Proteum (Version 1.35)'
_computing_data_reduction        'Siemens SAINT (V. 6.31a, Siemens 2002)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '5.602 pixels/mm'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15989
_diffrn_reflns_theta_full        59.46
_diffrn_reflns_theta_max         59.46
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.483
_exptl_absorpt_correction_T_max  0.8249
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0358P)^2^+1.0646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                3790
_reflns_number_total             4637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049605ksi20040602_052215.cif
_cod_data_source_block           3
_cod_original_cell_volume        3250(1)
_cod_database_code               4087352