The First Coordination Polymers and Hydrogen Bonded Networks Containing Octahedral Nb6 Clusters and Alkaline Earth Metal Complexes
Zhihua Yan; Cynthia S. Day; Abdessadek Lachgar; Inorganic Chemistry 44 (2005) 4499–4505; doi:10.1021/ic048453i

data_4309056
_publ_contact_author_address
; 
Department of Chemistry 
Wake Forest University 
Winston-Salem, N.C. 27109 
U.S.A. 
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         '336 758 4656'
_publ_contact_author_name        'Abdessadek Lachgar'
_publ_contact_author_phone       '336 758 4676'
_publ_section_title
;
The First Coordination Polymers and Hydrogen Bonded Networks Containing
Octahedral Nb6 Clusters and Alkaline Earth Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4499
_journal_page_last               4505
_journal_paper_doi               10.1021/ic048453i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C69.2 H61 Ca2 Cl12 N16 Nb6 O7'
_chemical_formula_weight         2291.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-PC
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5499(6)
_cell_length_b                   17.5305(8)
_cell_length_c                   21.7842(10)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.14
_cell_volume                     4331.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL-NT Ver. 6.12(Bruker, 2001)'
_computing_publication_material  'Bruker SHELXTL-NT Ver. 6.12(Bruker, 2001)'
_computing_structure_refinement  'Bruker SHELXTL-NT Ver. 6.12(Bruker, 2001)'
_computing_structure_solution    'Bruker SHELXTL-NT Ver. 6.12(Bruker, 2001)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76253
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.8582
_exptl_absorpt_correction_T_min  0.4349
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.594
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         30750
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          2.155
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.8799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                23794
_reflns_number_total             30750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048453isi20041104_095046_2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C69.20 H61 Ca2 Cl12 N16 Nb6 O7'
_cod_database_code               4309056