Dinitrogen Reduction by a Chromium(0) Complex Supported by a 16-Membered Phosphorus Macrocycle
Michael T. Mock; Shentan Chen; Molly O'Hagan; Roger Rousseau; William G. Dougherty; W. Scott Kassel; R. Morris Bullock; Journal of the American Chemical Society 135 (2013) 11493–11496; doi:10.1021/ja405668u

data_4120240
_publ_contact_author_address
;Center for Molecular Electrocatalysis
Pacific Northwest National Laboratory
P.O. Box 999, K2-57
Richland, Washington 99352
;
_publ_contact_author_email       michael.mock@pnnl.gov
_publ_contact_author_name        'Michael T. Mock'
_publ_section_title
;
 Dinitrogen Reduction by a Chromium(0) Complex Supported by a 16-Membered
 Phosphorus Macrocycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11493
_journal_page_last               11496
_journal_paper_doi               10.1021/ja405668u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H32 Cr0.5 N4 P2'
_chemical_formula_weight         536.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.117(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4009(12)
_cell_length_b                   16.1929(15)
_cell_length_c                   26.619(2)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.10
_cell_measurement_theta_min      2.49
_cell_volume                     5776.3(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.975
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            50425
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         34.16
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.9723
_exptl_absorpt_correction_T_min  0.9522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         11647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0506P)^2^+3.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                7721
_reflns_number_total             11647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405668u_si_001_1.cif
_cod_data_source_block           pnl114_all_syn_Cr(N2)2PPh4NBn4
_cod_original_cell_volume        5776.2(9)
_cod_original_formula_sum        'C30 H32 Cr0.50 N4 P2'
_cod_database_code               4120240