Short Intramolecular N-H...C(carbonyl) Interactions in Mixed-Ligand Molybdenum Hexacarbonyl Derivatives
Budge, Matthew G.; Muir, Kathleen J.; McQuillan, Geoffrey P.; Harrison, William T.A.; Crystals 1 (2012) 47–58; doi:10.3390/cryst1020047

data_1508405
_publ_section_title
;
 Short Intramolecular N-H...C(carbonyl) Interactions in Mixed-Ligand
 Molybdenum Hexacarbonyl Derivatives
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              47
_journal_page_last               58
_journal_paper_doi               10.3390/cryst1020047
_journal_volume                  1
_journal_year                    2012
_chemical_formula_moiety         'C24 H19 Mo N5 O3'
_chemical_formula_sum            'C24 H19 Mo N5 O3'
_chemical_formula_weight         521.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'difmap (N-H) and geom (C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.065(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4222(3)
_cell_length_b                   21.5966(9)
_cell_length_c                   12.5011(5)
_cell_measurement_reflns_used    6705
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.49
_cell_volume                     2268.12(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13657
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                3269
_reflns_number_total             3998
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file
C24H19MoN5O3_P21_n_crystals-01-00047-s001_moco3_DC150.CIF
_cod_data_source_block           gm005_chateigner_1508405
_cod_depositor_comments          'journal volume and issue reversed'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1508405