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_7705279
_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         '0.5(C54 H74 N6 Na4 O8)'
_chemical_formula_sum            'C27 H37 N3 Na2 O4'
_chemical_formula_weight         513.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-07 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.285(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.427(5)
_cell_length_b                   18.077(10)
_cell_length_c                   11.027(4)
_cell_measurement_reflns_used    281
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      3.07
_cell_volume                     2642(2)
_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
_diffrn_measured_fraction_theta_full 0.508
_diffrn_measured_fraction_theta_max 0.484
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.508
_diffrn_reflns_Laue_measured_fraction_max 0.484
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1939
_diffrn_reflns_point_group_measured_fraction_full 0.508
_diffrn_reflns_point_group_measured_fraction_max 0.484
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.300
_diffrn_reflns_theta_min         3.074
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1595
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_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                973
_reflns_number_total             1595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02692a2.cif
_cod_data_source_block           c2c_a
_cod_depositor_comments
'Adding full bibliography for 7705278--7705279.cif.'
_cod_original_cell_volume        2641.5(19)
_cod_database_code               7705279
_shelx_shelxl_version_number     2018/3
_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:
 C00E(H00E,H00F), C00F(H00G,H00H)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D), C00H(H00L)
2.c Idealised Me refined as rotating group:
 C00G(H00I,H00J,H00K), C00I(H00M,H00N,H00O), C00J(H00P,H00Q,H00R)
;
_shelx_res_checksum              10428
_olex2_submission_special_instructions 'No special instructions were received'