Crystal structure of (4-(4-chlorophenyl)-5-ethyl-1,3-dioxane-5-carboxylato-κ2 O,O′)-(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4 N,N′,N′′,N′′′)nickel(II) perchlorate monohydrate, C29H52Cl2N4NiO9
Liu, Fang; Jia, Guo-Kai; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 993–995; doi:10.1515/ncrs-2018-0095

data_8106374
_publ_section_title
;
 Crystal structure of
 (4-(4-chlorophenyl)-5-ethyl-1,3-dioxane-5-carboxylato-\k2
 O,O&#x2032;)-(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;)nickel(II)
 perchlorate monohydrate, C29H52Cl2N4NiO9
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              993
_journal_page_last               995
_journal_paper_doi               10.1515/ncrs-2018-0095
_journal_volume                  233
_journal_year                    2018
_chemical_formula_sum            'C29 H52 Cl2 N4 Ni O9'
_chemical_formula_weight         730.35
_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                 93.344(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8347(19)
_cell_length_b                   14.502(3)
_cell_length_c                   21.731(4)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.34
_cell_volume                     3408.7(11)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37399
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         1.689
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.7992
_exptl_absorpt_correction_T_min  0.7203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       peism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7623
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0515P)^2^+2.2315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6625
_reflns_number_total             7623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0095_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        3408.6(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8106374
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              72769
_shelx_hkl_checksum              68472