Steric Switching From Photochemical to Thermal Reaction Pathways for Enhanced Efficiency in Metal-Mediated Nitrogen Fixation.
Duman, Leila M.; Farrell, Wesley S.; Zavalij, Peter Y.; Sita, Lawrence R.; Journal of the American Chemical Society  (2016) –; doi:10.1021/jacs.6b09789

data_4125304
_publ_section_title
;
 Steric Switching From Photochemical to Thermal Reaction Pathways for
 Enhanced Efficiency in Metal-Mediated Nitrogen Fixation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.6b09789
_journal_year                    2016
_chemical_formula_moiety         'C42 H60 N6 W2'
_chemical_formula_sum            'C42 H60 N6 W2'
_chemical_formula_weight         1016.66
_chemical_name_systematic        W-complex
_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_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-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 91.9751(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9239(4)
_cell_length_b                   14.3150(7)
_cell_length_c                   16.5395(8)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.6
_cell_volume                     2111.59(17)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'XT/ShelXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0229738
_diffrn_orient_matrix_UB_12      -0.0353079
_diffrn_orient_matrix_UB_13      0.0511016
_diffrn_orient_matrix_UB_21      0.0217984
_diffrn_orient_matrix_UB_22      0.0600979
_diffrn_orient_matrix_UB_23      0.0289041
_diffrn_orient_matrix_UB_31      -0.1075597
_diffrn_orient_matrix_UB_32      0.0046466
_diffrn_orient_matrix_UB_33      0.0145991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.478
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1004
_exptl_crystal_id                'Sita-Leila LD-1-100'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.799
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+3.7350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5208
_reflns_number_total             6159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09789_si_002.cif
_cod_data_source_block           cmpd_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4125304
_shelx_estimated_absorpt_t_min   0.330
_shelx_estimated_absorpt_t_max   0.771
_shelx_res_checksum              52007
_shelx_hkl_checksum              2621