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_7124672
_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 F4 N6 P4 W'
_chemical_formula_sum            'C34 H58 F4 N6 P4 W'
_chemical_formula_weight         934.59
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2015-04-22
_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                 95.4260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2469(2)
_cell_length_b                   18.3292(3)
_cell_length_c                   21.5498(4)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.838
_cell_measurement_theta_min      2.291
_cell_volume                     4029.29(13)
_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    'XM (Sheldrick, 2008)'
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            206157
_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         36.318
_diffrn_reflns_theta_min         1.461
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_T_max  0.7339
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0622 before and 0.0585 after correction. The Ratio of minimum to maximum transmission is 0.7106. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethyl Ether'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.077
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.482(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         39026
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                35076
_reflns_number_total             39026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03449g2.cif
_cod_data_source_block           pnl190
_cod_database_code               7124672
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.518(3) 0.482(3)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C111(H11A,H11B), C113(H11F,H11G), C115(H11K,H11L), C116(H11M,H11N), C118(H11R,
 H11S), C120(H12A,H12B), C121(H12C,H12D), C128(H12E,H12F), C130(H13A,H13B),
 C132(H13F,H13G), C133(H13H,H13I), C135(H13M,H13N), C137(H13R,H13S), C138(H13T,
 H13U), C211(H21A,H21B), C213(H21F,H21G), C215(H21K,H21L), C216(H21M,H21N),
 C218(H21R,H21S), C220(H22A,H22B), C221(H22C,H22D), C228(H22E,H22F), C230(H23A,
 H23B), C232(H23F,H23G), C233(H23H,H23I), C235(H23M,H23N), C237(H23R,H23S),
 C238(H23T,H23U)
3.b Aromatic/amide H refined with riding coordinates:
 C124(H124), C125(H125), C126(H126), C141(H141), C142(H142), C143(H143),
 C224(H224), C225(H225), C226(H226), C241(H241), C242(H242), C243(H243)
3.c Idealised Me refined as rotating group:
 C112(H11C,H11D,H11E), C114(H11H,H11I,H11J), C117(H11O,H11P,H11Q), C119(H11T,
 H11U,H11V), C129(H12G,H12H,H12I), C131(H13C,H13D,H13E), C134(H13J,H13K,H13L),
 C136(H13O,H13P,H13Q), C212(H21C,H21D,H21E), C214(H21H,H21I,H21J), C217(H21O,
 H21P,H21Q), C219(H21T,H21U,H21V), C229(H22G,H22H,H22I), C231(H23C,H23D,H23E),
 C234(H23J,H23K,H23L), C236(H23O,H23P,H23Q)
;
_shelx_res_checksum              36012
_shelx_hkl_checksum              10250
_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'