Towards multicomponent MOFs via solvent-free synthesis under conventional oven and microwave assisted heating
Lanchas, Mónica; Arcediano, Sandra; Beobide, Garikoitz; Castillo, Oscar; Luque, Antonio; Pérez-Yáñez, Sonia; Inorganic Chemistry Frontiers 2 (2015) 425–; doi:10.1039/C4QI00208C

data_4348383
_publ_section_title
;
 Towards multicomponent MOFs via solvent-free synthesis under conventional
 oven and microwave assisted heating
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              425
_journal_paper_doi               10.1039/C4QI00208C
_journal_volume                  2
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C14 H18 N10 Ni2 O10, 2(C5 H6 N5), 2(H C O2), 2(H2 C O2)'
_chemical_formula_structural
'C14 H18 N10 Ni2 O10, 2(C5 H6 N5), 2(H C O2), 2(H2 C O2)'
_chemical_formula_sum            'C28 H36 N20 Ni2 O18'
_chemical_formula_weight         1058.19
_chemical_name_systematic
'[bis(mu-adenine-kN3:kN9)diaquabis(mu-formato-kO:kO)bisformatodinickel(II)]-adeninium formate-formic acid (1/2/2)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_audit_update_record
;
2014-11-21 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                114.763(5)
_cell_angle_beta                 100.349(5)
_cell_angle_gamma                100.859(5)
_cell_formula_units_Z            1
_cell_length_a                   7.1579(4)
_cell_length_b                   12.8195(7)
_cell_length_c                   13.0602(7)
_cell_measurement_reflns_used    7105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.79
_cell_volume                     1022.83(12)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7105
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.8582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                3531
_reflns_number_total             4359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00208c2.cif
_cod_data_source_block           compound-4
_cod_original_cell_volume        1022.83(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348383