Reactions of Grignard Reagents with Nitrous Oxide
Tskhovrebov, Alexander G.; Solari, Euro; Scopelliti, Rosario; Severin, Kay; Organometallics 33 (2014) 2405–; doi:10.1021/om500333y

data_4083179
_publ_section_title
;
 Reactions of Grignard Reagents with Nitrous Oxide
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2405
_journal_paper_doi               10.1021/om500333y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C32 H64 Cl4 Mg5 N4 O6'
_chemical_formula_sum            'C32 H64 Cl4 Mg5 N4 O6'
_chemical_formula_weight         864.22
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-02-10 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.705(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.483(2)
_cell_length_b                   18.8942(15)
_cell_length_c                   21.2253(17)
_cell_measurement_reflns_used    691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     4524.9(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61326
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         12819
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+3.9321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                10042
_reflns_number_total             12819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500333y_si_002.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
'Adding full bibliography for 4083179--4083181.cif.'
_cod_original_cell_volume        4525.1(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4083179