Dinitrogen activation by a penta-pyridyl molybdenum complex.
Cha, Jeongmin; Kwon, Hyunchul; Song, Hayoung; Lee, Eunsung; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12945–12949; doi:10.1039/d0dt02692a

data_7705278
_publ_section_title
;
 Dinitrogen activation by a penta-pyridyl molybdenum complex.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12945
_journal_page_last               12949
_journal_paper_doi               10.1039/d0dt02692a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H25 Mo N7'
_chemical_formula_sum            'C29 H25 Mo N7'
_chemical_formula_weight         567.50
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.307(3)
_cell_length_b                   11.256(2)
_cell_length_c                   20.349(4)
_cell_measurement_reflns_used    1781
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      2.511
_cell_volume                     3277.0(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       phi-scan
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3254
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.511
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull violet'
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.963
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+38.9779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1706
_reflns_number_total             1781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02692a2.cif
_cod_data_source_block           cmc21
_cod_depositor_comments
'Adding full bibliography for 7705278--7705279.cif.'
_cod_original_cell_volume        3277.0(12)
_cod_database_code               7705278
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C10, C6, C4, C2, C1, C5, C9, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C6 \\sim C4 \\sim C2 \\sim C1 \\sim C5 \\sim C9 \\sim C7 \\sim C8:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5) = Uanis(C4)
Uanis(N3) = Uanis(N1)
Uanis(C8) = Uanis(C2)
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C2(H2), C9(H9), C7(H7), C8(H8)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'