Synthesis and structures of urea-coordinated dinickel(II) complexes with binucleating ligand 1,3-bis(N-(2-(dimethylamino)ethyl)-N-methylamino)propan-2-ol (HL1) and its a nalogs
Katsura Mochizuki; Junpei Takahashi; Yukiko Ishima; Tomomi Shindo; Inorganica Chimica Acta 400 (2013) 151–158; doi:

data_1516929
_publ_section_title
;
 Synthesis and structures of urea-coordinated dinickel(II) complexes with
 binucleating ligand
 1,3-bis(N-(2-(dimethylamino)ethyl)-N-methylamino)propan-2-ol (HL1) and
 its a nalogs
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              151
_journal_page_last               158
_journal_volume                  400
_journal_year                    2013
_chemical_formula_sum            'C46 H73 B N6 Ni2 O8'
_chemical_formula_weight         966.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.69(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.591(8)
_cell_length_b                   17.449(5)
_cell_length_c                   17.256(7)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.41
_cell_measurement_theta_min      15.07
_cell_volume                     5124(4)
_computing_cell_refinement       'MXC (MAC Science)'
_computing_data_collection       'MXC (MAC Science)'
_computing_data_reduction        'MXC (MAC Science)'
_computing_molecular_graphics    Ortep-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir-92 in MAXUS'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Mac Science MXC3k'
_diffrn_measurement_method       Omega
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12087
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular Solid'
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.068
_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     569
_refine_ls_number_reflns         11712
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0670P)^2^+4.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                7365
_reflns_number_total             11712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-400-151-158-2.cif
_cod_data_source_block           5a+urea-EtOH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Psi-Scan' changed to
'psi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1516929