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_7034465
_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         'C196 H270 Ca2 N8 O35'
_chemical_formula_sum            'C196 H270 Ca2 N8 O35'
_chemical_formula_weight         3378.34
_chemical_name_systematic
; 
 [{[(t-BuC6H4)3CCONH](n-BuCONH)C6H3COO}4Ca2(H2O)5(dioxane)]-4(dioxane)-4(H2O)
;
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.006(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.0688(18)
_cell_length_b                   11.3006(12)
_cell_length_c                   50.441(5)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     9795.0(18)
_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    'SHELXS-97 (Sheldrick, 2008)'
_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  0.2746
_diffrn_reflns_av_unetI/netI     0.2513
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            73841
_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         24.999
_diffrn_reflns_theta_min         3.044
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3644
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         17222
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.3361
_refine_ls_R_factor_gt           0.1481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3610
_refine_ls_wR_factor_ref         0.4705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5008
_reflns_number_total             17222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00053j2.cif
_cod_data_source_block           Ca2L24-4(1,4-dioxane)-4H2O
_cod_depositor_comments
'Adding full bibliography for 7034462--7034467.cif.'
_cod_original_cell_volume        9795.1(18)
_cod_database_code               7034465
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014/6