Crystal structure of [(μ2-succinato κ3 O,O′:O′′)-bis-(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)]dinickel(II)] diperchlorate, dihydrate C36H82Cl2N8Ni2O15
Li, Wen-Yi; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 491–493; doi:10.1515/ncrs-2020-0616

data_8104747
_publ_section_title
;
 Crystal structure of [(\m2-succinato \k3
 O,O&#x2032;:O&#x2032;&#x2032;)-bis-(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)]dinickel(II)]
 diperchlorate, dihydrate C36H82Cl2N8Ni2O15
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              491
_journal_page_last               493
_journal_paper_doi               10.1515/ncrs-2020-0616
_journal_volume                  236
_journal_year                    2021
_chemical_formula_sum            'C36 H82 Cl2 N8 Ni2 O15'
_chemical_formula_weight         1055.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 109.062(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.657(3)
_cell_length_b                   16.047(3)
_cell_length_c                   18.346(3)
_cell_measurement_reflns_used    2907
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.54
_cell_volume                     4913.2(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21783
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.034
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.8263
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.210
_exptl_transmission_factor_max   0.826
_exptl_transmission_factor_min   0.698
_refine_diff_density_max         1.821
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10493
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0827P)^2^+5.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6805
_reflns_number_total             10493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0616_suppl.cif
_cod_data_source_block           L801122m
_cod_original_cell_volume        4913.2(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8104747
_shelx_estimated_absorpt_t_min   0.698
_shelx_estimated_absorpt_t_max   0.826