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_4120241
_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            'C34 H40 Cl Cr0.5 N2 O P2'
_chemical_formula_weight         616.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.617(3)
_cell_angle_beta                 78.022(3)
_cell_angle_gamma                71.001(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0093(5)
_cell_length_b                   13.4763(8)
_cell_length_c                   14.3888(9)
_cell_measurement_reflns_used    4384
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      2.65
_cell_volume                     1520.36(16)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.1897
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24148
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.24
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.9501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         11613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1708
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0098P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                5602
_reflns_number_total             11613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405668u_si_001_2.cif
_cod_data_source_block           pnl081_syn_anti_anti_CrCl2PPh4NBn4
_cod_original_formula_sum        'C34 H40 Cl Cr0.50 N2 O P2'
_cod_database_code               4120241