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_4120243
_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            'C45 H48 Cl3 Cr N3 P3'
_chemical_formula_weight         882.12
_chemical_name_systematic
; 
 ? 
;
_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                 96.408(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5327(11)
_cell_length_b                   15.5382(12)
_cell_length_c                   17.1832(13)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.27
_cell_measurement_theta_min      3.11
_cell_volume                     4121.3(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-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 0.998
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70257
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.28
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.8850
_exptl_absorpt_correction_T_min  0.8850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       rod
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         15836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.7388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                13640
_reflns_number_total             15836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405668u_si_001_4.cif
_cod_data_source_block           pnl088_CrCl3PPh3NBn3
_cod_database_code               4120243