Systematic Variation of Metal-Metal Bond Order in Metal-Chromium Complexes
Laura J. Clouston; Randall B. Siedschlag; P. Alex Rudd; Nora Planas; Shuxian Hu; Adam D. Miller; Laura Gagliardi; Connie C. Lu; Journal of the American Chemical Society 135 (2013) 13142–13148; doi:10.1021/ja406506m

data_4120720
_publ_section_title
;
 Systematic Variation of Metal-Metal Bond Order in Metal-Chromium
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13142
_journal_page_last               13148
_journal_paper_doi               10.1021/ja406506m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C39 H60 Cr Mn N4 P3'
_chemical_formula_sum            'C39 H60 Cr Mn N4 P3'
_chemical_formula_weight         784.76
_chemical_name_common            MnCrL
_space_group_IT_number           150
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.9786(18)
_cell_length_b                   15.9786(18)
_cell_length_c                   11.6916(13)
_cell_measurement_reflns_used    4462
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.235
_cell_measurement_theta_min      2.281
_cell_volume                     2585.1(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12767
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.8942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Squeeze results consistent with 3 disordered THF molecules
;
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                3040
_reflns_number_total             3922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406506m_si_004.cif
_cod_data_source_block           12212sq
_cod_database_code               4120720