Synthesis and Crystal Structure of a Nickel(II) Complex with 1,3-Bis(pyrrole-2-methylideneamino)-2-propanol
MIKURIYA, Masahiro; HARA, Masashi; YOSHIOKA, Daisuke; X-ray Structure Analysis Online 33 (2017) 59–; doi:10.2116/xraystruct.33.59

data_1551583
_publ_section_title
;
 Synthesis and Crystal Structure of a Nickel(II) Complex with
 1,3-Bis(pyrrole-2-methylideneamino)-2-propanol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              59
_journal_paper_doi               10.2116/xraystruct.33.59
_journal_volume                  33
_journal_year                    2017
_chemical_formula_sum            'C13.5 H16 N4 Ni O1.5'
_chemical_formula_weight         317.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                94.036(2)
_cell_angle_beta                 108.801(2)
_cell_angle_gamma                104.820(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6947(12)
_cell_length_b                   12.0269(15)
_cell_length_c                   13.2626(18)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.566
_cell_measurement_theta_min      1.645
_cell_volume                     1395.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9019
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.566
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4093
_reflns_number_total             6384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_59_1.txt
_cod_data_source_block           Ni4211m_0m
_cod_original_formula_sum        'C13.50 H16 N4 Ni O1.50'
_cod_database_code               1551583
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.768
_shelx_res_checksum              4206
_shelx_hkl_checksum              30449