Structural Variability and Dynamics in Carboxylato- and Carbamatomagnesium Bromides. Relationship to the Carboxylate Shift
M. Tyler Caudle; William W. Brennessel; Victor G. Young; Inorganic Chemistry 44 (2005) 3233–3240; doi:10.1021/ic048442p

data_4308815
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
Arizona State University
College of Liberal Arts and Sciences
P.O. Box 871604
Tempe, AZ, 85287-1604
;
_publ_contact_author_email       Tcaudle@asu.edu
_publ_contact_author_fax         '480 965 2747'
_publ_contact_author_name        'Professor Tyler Caudle'
_publ_contact_author_phone       '480 965 5178'
_publ_section_title
;
Structural Variability and Dynamics in Carboxylato- and Carbamatomagnesium
Bromides. Relationship to the Carboxylate Shift
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3233
_journal_page_last               3240
_journal_paper_doi               10.1021/ic048442p
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
'C4 H8 O, C4 H8 Br3 Mg O, C72 H80 Br Mg3 N4 O13'
_chemical_formula_sum            'C80 H96 Br4 Mg4 N4 O15'
_chemical_formula_weight         1770.49
_chemical_name_common            00038
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.387(1)
_cell_angle_beta                 92.529(2)
_cell_angle_gamma                102.686(1)
_cell_formula_units_Z            2
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_cell_length_b                   13.981(1)
_cell_length_c                   23.562(2)
_cell_measurement_reflns_used    5345
_cell_measurement_temperature    173(2)
_cell_volume                     4190.8(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29326
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.830655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         14677
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0919P)^2^+0.5900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                10345
_reflns_number_total             14677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048442psi20041105_075201.cif
_cod_data_source_block           00038
_cod_original_cell_volume        4190.7(6)
_cod_database_code               4308815