Putting chromium on the map for N2 reduction: production of hydrazine and ammonia. A study of cis-M(N2)2 (M = Cr, Mo, W) bis(diphosphine) complexes.
Egbert, Jonathan D.; O'Hagan, Molly; Wiedner, Eric S.; Bullock, R. Morris; Piro, Nicholas A.; Kassel, W. Scott; Mock, Michael T.; Chemical communications (Cambridge, England) 52 (2016) 9343–9346; doi:10.1039/c6cc03449g

data_7124671
_publ_section_title
;
 Putting chromium on the map for N2 reduction: production of hydrazine and
 ammonia. A study of cis-M(N2)2 (M = Cr, Mo, W) bis(diphosphine)
 complexes.
;
_journal_issue                   60
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9343
_journal_page_last               9346
_journal_paper_doi               10.1039/c6cc03449g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C34 H58 Cr F4 N6 P4'
_chemical_formula_sum            'C34 H58 Cr F4 N6 P4'
_chemical_formula_weight         802.74
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-05 deposited with the CCDC.
2016-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3010(2)
_cell_length_b                   18.8047(4)
_cell_length_c                   20.7192(4)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.837
_cell_measurement_theta_min      2.166
_cell_volume                     4004.77(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            92748
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.464
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8876.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethyl Ether'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         11730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+1.6094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8640
_reflns_number_total             11730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03449g2.cif
_cod_data_source_block           pnl189
_cod_database_code               7124671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C21(H21A,H21B), C27(H27A,H27B), C10(H10A,H10B), C28(H28A,
 H28B), C11(H11A,H11B), C25(H25A,H25B), C19(H19A,H19B), C9(H9A,H9B), C1(H1A,
 H1B), C23(H23A,H23B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C33(H33), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              14091
_shelx_hkl_checksum              58716
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'mounted in NVH imersion oil on a nylon fiber'
_olex2_submission_special_instructions 'No special instructions were received'