Synthesis and reactivity of an N-triphos Mo(0) dinitrogen complex.
Apps, Samantha L.; White, Andrew J. P.; Miller, Philip W.; Long, Nicholas J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11386–11396; doi:10.1039/c8dt02471e

data_7047092
_publ_section_title
;
 Synthesis and reactivity of an N-triphos Mo(0) dinitrogen complex.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11386
_journal_page_last               11396
_journal_paper_doi               10.1039/c8dt02471e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C64 H58 Mo N P5, B C24 F20, C6 H5 F'
_chemical_formula_sum            'C94 H63 B F21 Mo N P5'
_chemical_formula_weight         1867.05
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1523(4)
_cell_length_b                   40.9129(12)
_cell_length_c                   15.2959(4)
_cell_measurement_reflns_used    7168
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.7650
_cell_measurement_theta_min      2.4500
_cell_volume                     8220.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27499
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.832
_diffrn_reflns_theta_min         2.492
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plates
_exptl_crystal_F_000             3780
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.748
_exptl_crystal_size_mid          0.428
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         16056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0263P)^2^+9.6133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12592
_reflns_number_total             16056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02471e2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7047089--7047092.cif.'
_cod_database_code               7047092
_shelx_shelxl_version_number     2017/1
_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. Restrained distances
 N1-H1
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C59(H59), C17(H17), C77(H77), C61(H61), C15(H15), C64(H64),
 C18(H18), C63(H63), C25(H25), C16(H16), C58(H58), C71(H71), C13(H13), C73(H73),
  C65(H65), C27(H27), C43(H43), C62(H62), C68(H68), C36(H36), C35(H35),
 C19(H19), C67(H67), C11(H11), C75(H75), C33(H33), C41(H41), C31(H31), C69(H69),
  C9(H9), C34(H34), C74(H74), C55(H55), C37(H37), C115(H115), C42(H42),
 C56(H56), C76(H76), C28(H28), C12(H12), C70(H70), C24(H24), C57(H57), C23(H23),
  C29(H29), C10(H10), C30(H30), C40(H40), C113(H113), C114(H114), C22(H22),
 C39(H39), C112(H112), C111(H111)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              58676
_olex2_submission_special_instructions 'No special instructions were received'