Synthesis and structures of soluble magnesium and zinc carboxylates containing intramolecular NHO hydrogen bonds in nonpolar solvents.
Okamura, Taka-Aki; Furuya, Ryosuke; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7512–7523; doi:10.1039/c5dt00053j

data_7034462
_publ_section_title
;
 Synthesis and structures of soluble magnesium and zinc carboxylates
 containing intramolecular NHO hydrogen bonds in nonpolar solvents.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7512
_journal_page_last               7523
_journal_paper_doi               10.1039/c5dt00053j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C83 H108 N2 O10'
_chemical_formula_sum            'C83 H108 N2 O10'
_chemical_formula_weight         1293.71
_chemical_name_systematic
; 
[{t-BuC6H4)3CCONH}2C6H3COOH]-3(AcOEt) 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-04
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-01-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.968(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9473(8)
_cell_length_b                   13.9306(6)
_cell_length_c                   28.662(2)
_cell_measurement_reflns_used    14201
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.01
_cell_volume                     7509.4(7)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28924
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.011
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         13050
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1485P)^2^+1.6883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10640
_reflns_number_total             13050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00053j2.cif
_cod_data_source_block           L0H-3(AcOEt)
_cod_depositor_comments
'Adding full bibliography for 7034462--7034467.cif.'
_cod_database_code               7034462
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2014/6