Coordination polymers of a dipyridylazacrown ligand: structural, thermal and spectroscopic properties
Gee, William J.; Moubaraki, Boujemaa; Murray, Keith S.; Batten, Stuart R.; CrystEngComm 15 (2013) 9655–; doi:10.1039/c3ce41202d

data_7211074
_publ_section_title
;
 Coordination polymers of a dipyridylazacrown ligand: structural, thermal
 and spectroscopic properties
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9655
_journal_paper_doi               10.1039/c3ce41202d
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C48 H78 N8 Ni O10, 4(Cl O4), O, 3(H2 O)'
_chemical_formula_sum            'C48 H84 Cl4 N8 Ni O30'
_chemical_formula_weight         1453.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.576(4)
_cell_length_b                   14.207(3)
_cell_length_c                   25.869(5)
_cell_measurement_reflns_used    58514
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      1.16
_cell_volume                     6431(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Australian synchrotron MX1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1551
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58514
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            olive-green
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         16085
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1746
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+20.7792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                8461
_reflns_number_total             16085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41202d.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7211074