Solid-state coexistence of {Zr12} and {Zr6} zirconium oxocarboxylate clusters
Malaestean, Iurie L.; Alıcı, Meliha Kutluca; Besson, Claire; Ellern, Arkady; Kögerler, Paul; CrystEngComm 16 (2014) 43–; doi:10.1039/c3ce41829d

data_7214101
_publ_section_title
;
 Solid-state coexistence of {Zr12} and {Zr6} zirconium oxocarboxylate
 clusters
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              43
_journal_paper_doi               10.1039/c3ce41829d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C174 H287 Co8 N21 O119 Zr18'
_chemical_formula_weight         6690.63
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 123.6880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.819(4)
_cell_length_b                   31.046(3)
_cell_length_c                   28.384(5)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.35
_cell_volume                     26997(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.868
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            97371
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.999
_diffrn_reflns_theta_min         0.934
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             13464
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.660
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1568
_refine_ls_number_reflns         21198
_refine_ls_number_restraints     735
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+1060.0345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14830
_reflns_number_total             21198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41829d.txt
_cod_data_source_block           Kut005
_cod_original_cell_volume        26996(6)
_cod_database_code               7214101
_shelx_estimated_absorpt_t_min   0.757
_shelx_estimated_absorpt_t_max   0.847
_shelxl_version_number           2013-3
_shelx_res_checksum              24806
_shelx_hkl_checksum              77259