Transition metal dipicolinates as designer T-shaped building blocks
Felloni, Marina; Blake, Alexander J.; Hubberstey, Peter; Teat, Simon J.; Wilson, Claire; Schröder, Martin; CrystEngComm 12 (2010) 1576–; doi:10.1039/b915440j

data_7211839
_publ_section_title
;
 Transition metal dipicolinates as designer T-shaped building blocks
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1576
_journal_paper_doi               10.1039/b915440j
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C17 H11 Ni N5 O4, 0.5(C10 H8 N4), H2 O'
_chemical_formula_sum            'C22 H17 N7 Ni O5'
_chemical_formula_weight         518.14
_chemical_name_common            '[Ni(II)(dipic)(diazobpe)](H2O)(diazobpe)0.5'
_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
'aromatic H geometrically placed, water H located from delta-F'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   'difference Fourier method'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.310(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1967(7)
_cell_length_b                   15.8470(8)
_cell_length_c                   10.6187(5)
_cell_measurement_reflns_used    5646
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.26
_cell_volume                     2184.81(19)
_computing_cell_refinement       'Bruker SAINT version 6.02A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction
'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL/PC v.5.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97; PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6900
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.049
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15706
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.52
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment
'aromatic H refined with riding model, water H refined with restraints'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0357P)^2^+1.8784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4595
_reflns_number_total             6009
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b915440j.txt
_cod_data_source_block           NIDPEN_Complex_8
_cod_original_cell_volume        2184.8(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7211839