Lactam/MoCl5 interaction in CH2Cl2: synthesis and X-ray characterization of protonated δ-valerolactam salts
Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; RSC Advances 3 (2013) 10007–; doi:10.1039/c3ra23305g

data_7238929
_publ_section_title
;
 Lactam/MoCl5 interaction in CH2Cl2: synthesis and X-ray characterization
 of protonated \d-valerolactam salts
;
_journal_issue                   25
_journal_name_full               'RSC Advances'
_journal_page_first              10007
_journal_paper_doi               10.1039/c3ra23305g
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C11 H22 Cl7 Mo N2 O3'
_chemical_formula_weight         574.40
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.729(3)
_cell_length_b                   14.865(3)
_cell_length_c                   7.6628(13)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5635
_cell_measurement_theta_min      2.175
_cell_volume                     2133.4(7)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPIII (johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14718
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  0.8520
_exptl_absorpt_correction_T_min  0.7735
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.0628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                2208
_reflns_number_total             2410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra23305g.txt
_cod_data_source_block           pnma
_cod_original_cell_volume        2133.3(6)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7238929