Redetermination of the crystal structure of the 2D heterometallic framework prepared from [Ni(cyclam)]2+ and [Re(CN)7]3-
Sukhikh, Taisiya S.; Vostrikova, Kira E.; Journal of Solid State Chemistry 258 (2018) 485–487; doi:10.1016/j.jssc.2017.11.016

data_1561256
_publ_section_title
;
 Redetermination of the crystal structure of the 2D heterometallic
 framework prepared from [Ni(cyclam)]2+ and [Re(CN)7]3-
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              485
_journal_page_last               487
_journal_paper_doi               10.1016/j.jssc.2017.11.016
_journal_volume                  258
_journal_year                    2018
_chemical_formula_moiety
'0.5(C49 H96 N24 Ni4 O4 Re2), 2.5(Cl O4),  2.5(H2 O), C H4 O'
_chemical_formula_sum            'C25.5 H57 Cl2.5 N12 Ni2 O15.5 Re'
_chemical_formula_weight         1172.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2674(5)
_cell_length_b                   15.2674(5)
_cell_length_c                   19.4380(8)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.48
_cell_volume                     4530.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53370
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.754
_diffrn_reflns_theta_min         1.886
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0456 before and 0.0370 after correction. The Ratio of minimum to maximum transmission is 0.8893. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             2330
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4336
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+40.0380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3369
_reflns_number_total             4336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-258-485.cif
_cod_data_source_block           kv231a_1_2
_cod_original_cell_volume        4530.9(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C25.50 H57 Cl2.50 N12 Ni2 O15.50 Re'
_cod_database_code               1561256
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.625
_olex2_refinement_description
;
1. Restrained distances
 Cl41-O44 = Cl41-O46 = Cl41-O47 = Cl41-O45
 1.43 with sigma of 0.02
 Cl41-O42 = Cl41-O44 = Cl41-O43 = Cl41-O41
 1.43 with sigma of 0.02
 Cl51-O51 = Cl51-O52 = Cl51-O53 = Cl51-O54
 1.43 with sigma of 0.002
 O42-O43
 2.34 with sigma of 0.04
 O42-O41
 2.34 with sigma of 0.04
 O43-O41
 2.34 with sigma of 0.04
 O44-O45
 2.34 with sigma of 0.04
 O44-O46
 2.34 with sigma of 0.04
 O44-O47
 2.34 with sigma of 0.04
 O46-O47
 2.34 with sigma of 0.04
 O45-O47
 2.34 with sigma of 0.04
 O45-O46
 2.34 with sigma of 0.04
 O44-O42
 2.34 with sigma of 0.04
 O44-O43
 2.34 with sigma of 0.04
 O44-O41
 2.34 with sigma of 0.04
 O51-O52
 2.34 with sigma of 0.04
 O52-O53
 2.34 with sigma of 0.04
 O54-O51
 2.34 with sigma of 0.04
 O54-O52
 2.34 with sigma of 0.04
 O51-O53
 2.34 with sigma of 0.04
 O54-O53
 2.34 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uiso(O45) = Uiso(O41) = Uiso(O47) = Uiso(O43) = Uiso(O46) = Uiso(O42)
Uiso(O4S) = Uiso(O3S)
Uanis(O13) = Uanis(O12)
Uiso(O54) = Uiso(O51) = Uiso(O52) = Uiso(O53)
3. Others
 Fixed Sof: O13(0.25) C13(0.25) O45(0.5) O46(0.5) O47(0.5) O51(0.25) O41(0.5)
 O2S(0.5) O3S(0.5) O4S(0.5) O12(0.25) O43(0.5) O42(0.5) C3S(0.5) O54(0.25)
 O52(0.25) O53(0.25)
 Fixed Uiso: H21(0.02) H22(0.02) H31(0.02) H32(0.02) H21A(0.029) H21B(0.029)
 H21C(0.03) H21D(0.025) H21E(0.015) H21F(0.015) H21G(0.015) H21H(0.015)
 H21I(0.025) H21J(0.029) H31A(0.025) H31B(0.025) H31C(0.025) H31D(0.025)
 H31E(0.015) H31F(0.015) H31G(0.026) H31H(0.028) H31I(0.025) H31J(0.025)
4.a Ternary CH refined with riding coordinates:
 N21(H21), N22(H22), N31(H31), N32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C210(H21A,H21B), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J), C310(H31A,H31B), C311(H31C,H31D), C312(H31E,H31F), C313(H31G,H31H),
 C314(H31I,H31J)
;
_shelx_res_checksum              37681
_shelx_hkl_checksum              14503