Novel 3D Alkali‒Lanthanide Heterometal‒Organic Frameworks with Pyrazine-2,3,5,6-tetracarboxylic Acid: Synthesis, Structure, and Magnetism
Zhang, Fengming; Yan, Pengfei; Zou, Xiaoyan; Zhang, Juwen; Hou, Guangfeng; Li, Guangming; Crystal Growth & Design 14 (2014) 2014–; doi:10.1021/cg5001254

data_4510464
_publ_section_title
;
 Novel 3D Alkali--Lanthanide Heterometal--Organic Frameworks with
 Pyrazine-2,3,5,6-tetracarboxylic Acid: Synthesis, Structure, and
 Magnetism
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2014
_journal_paper_doi               10.1021/cg5001254
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C40 Ho5 N10 O50, 16(O), 5(K)'
_chemical_formula_sum            'C40 H52 Ho5 K5 N10 O66'
_chemical_formula_weight         2749.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   15.203(3)
_cell_length_b                   33.371(7)
_cell_length_c                   14.395(3)
_cell_measurement_reflns_used    45911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.03
_cell_volume                     7303(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52262
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.783
_exptl_absorpt_correction_T_max  0.5687
_exptl_absorpt_correction_T_min  0.4580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         6530
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0355P)^2^+31.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                4923
_reflns_number_total             6530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5001254_si_003.cif
_cod_data_source_block           Ho
_cod_database_code               4510464