Crystal structure of (dimethylformamide-κO)(perchlorato-κ2 O,O′){μ2-6,6′-((1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-methoxyphenolate)-κ8 N,N′,O:O,O′:O′,O′′,O′′′}sodium(I)nickel(II), C25H23Br2ClN3NaNiO9
Meng, Qingguo; Yue, Chen; Yu, Jiangkun; Liu, Qingyun; Lu, Jitao; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 409–411; doi:10.1515/ncrs-2017-0309

data_8106167
_publ_section_title
;
 Crystal structure of (dimethylformamide-\kO)(perchlorato-\k2
 O,O&#x2032;){\m2-6,6&#x2032;-((1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-methoxyphenolate)-\k8
 N,N&#x2032;,O:O,O&#x2032;:O&#x2032;,O&#x2032;&#x2032;,O&#x2032;&#x2032;&#x2032;}sodium(I)nickel(II),
 C25H23Br2ClN3NaNiO9
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              409
_journal_page_last               411
_journal_paper_doi               10.1515/ncrs-2017-0309
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C25 H23 Br2 Cl N3 Na Ni O9'
_chemical_formula_sum            'C25 H23 Br2 Cl N3 Na Ni O9'
_chemical_formula_weight         786.43
_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   geom
_cell_angle_alpha                90
_cell_angle_beta                 114.536(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.595(4)
_cell_length_b                   10.993(3)
_cell_length_c                   18.660(5)
_cell_measurement_reflns_used    1865
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.519
_cell_measurement_theta_min      2.651
_cell_volume                     2910.1(13)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)[9]'
_computing_data_collection       'SAINT-Plus (Bruker, 2001)[9]'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)[9]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[10]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[10]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[11]'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)[11]'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.681
_diffrn_reflns_theta_min         2.207
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.6944
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.1977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3992
_reflns_number_total             6678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0309_suppl.cif
_cod_data_source_block           test
_cod_original_cell_volume        2910.2(14)
_cod_database_code               8106167
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-N3 \\sim N3-C24A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C24A, C24, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C24A(0.5) H24D(0.5)
 H24E(0.5) H24F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C18(H18),
 C20(H20), C21(H21), C23(H23)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              32895
_shelx_hkl_checksum              19327
_olex2_submission_special_instructions 'No special instructions were received'