The crystal structure and oxygen reduction reaction of Ni(ii)-complex templated borate-sulfate and borate
Xin, Shu-Sheng; Deng, Yan-Ling; Pan, Chun-Yang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00213B

data_7709862
_publ_section_title
;
 The crystal structure and oxygen reduction reaction of Ni(ii)-complex
 templated borate-sulfate and borate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00213B
_journal_year                    2022
_chemical_formula_moiety         'C12 H24 N6 Ni O3, 2(B5 H4 O10)'
_chemical_formula_sum            'C12 H32 B10 N6 Ni O23'
_chemical_formula_weight         795.24
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-21 deposited with the CCDC.	2022-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8428(3)
_cell_length_b                   11.2042(2)
_cell_length_c                   33.9565(7)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.17
_cell_volume                     6585.4(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            92669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_min         1.920
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.4058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         13456
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0521P)^2^+4.4924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10627
_reflns_number_total             13456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00213b2.cif
_cod_data_source_block           mo_1215_3_0m
_cod_database_code               7709862
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00C(0.051) H00I(0.05) H00M(0.047) H00O(0.047) H00P(0.049)
 H00V(0.049) H00X(0.051) H00Y(0.053) H00A(0.052) H00B(0.052) H01A(0.051)
 H01B(0.051) H011(0.051) H012(0.052) H013(0.05) H014(0.054) H015(0.053)
 H016(0.055) H01H(0.053) H01I(0.053) H018(0.057) H019(0.058) H01J(0.054)
 H01K(0.054) H01C(0.058) H01D(0.058) H01L(0.062) H01M(0.062) H01P(0.043)
 H01Q(0.048) H01R(0.042) H01S(0.039) H01T(0.047) H01E(0.065) H01F(0.065)
 H01G(0.065) H01V(0.047) H01W(0.042) H01N(0.067) H01O(0.067) H01U(0.067)
 H01Y(0.05) H01Z(0.051) H020(0.044) H022(0.056) H023(0.055) H024(0.052)
 H02H(0.072) H02I(0.072) H02J(0.072) H02A(0.075) H02B(0.075) H02C(0.075)
 H028(0.053) H029(0.064) H02D(0.057) H02E(0.08) H02F(0.08) H02G(0.08)
 H02Q(0.054) H02V(0.059) H02K(0.09) H02L(0.09) H02M(0.09)
 Fixed X: H00C(0.714342) H00I(0.783573) H00M(1.079093) H00O(-0.075655)
 H00P(0.422327) H00V(0.206642) H00X(0.064571) H00Y(0.575479) H00A(0.761565)
 H00B(0.802164) H01A(0.737785) H01B(0.692729) H011(0.948653) H012(0.42664)
 H013(0.293361) H014(0.578639) H015(0.435391) H016(1.072487) H01H(0.762531)
 H01I(0.805721) H018(0.545774) H019(-0.077451) H01J(0.732899) H01K(0.693045)
 H01C(0.756479) H01D(0.691483) H01L(0.713135) H01M(0.789318) H01P(0.732209)
 H01Q(0.907224) H01R(0.772349) H01S(0.886616) H01T(0.585527) H01E(1.073659)
 H01F(1.083818) H01G(1.02623) H01V(0.585078) H01W(0.615451) H01N(0.429401)
 H01O(0.416671) H01U(0.477877) H01Y(0.730169) H01Z(1.039191) H020(0.612224)
 H022(0.722987) H023(0.912405) H024(0.456052) H02H(0.715302) H02I(0.805904)
 H02J(0.774462) H02A(0.473153) H02B(0.40933) H02C(0.434409) H028(0.454482)
 H029(0.770607) H02D(0.767895) H02E(0.73699) H02F(0.789434) H02G(0.697412)
 H02Q(0.883235) H02V(1.042596) H02K(1.021567) H02L(1.084306) H02M(1.065922)
 Fixed Y: H00C(0.682016) H00I(0.753504) H00M(0.427422) H00O(1.014377)
 H00P(0.482759) H00V(0.689676) H00X(0.704368) H00Y(0.43101) H00A(0.591946)
 H00B(0.490474) H01A(0.640573) H01B(0.539427) H011(0.744375) H012(1.01009)
 H013(0.749636) H014(0.960855) H015(0.705689) H016(0.954548) H01H(0.697241)
 H01I(0.594352) H018(0.741254) H019(0.486841) H01J(0.663091) H01K(0.559616)
 H01C(0.361497) H01D(0.360263) H01L(0.394834) H01M(0.393137) H01P(0.815583)
 H01Q(0.616744) H01R(0.866625) H01S(0.522589) H01T(0.679851) H01E(0.45896)
 H01F(0.599682) H01G(0.525925) H01V(0.656876) H01W(0.57925) H01N(0.513318)
 H01O(0.653662) H01U(0.58391) H01Y(1.067862) H01Z(0.602552) H020(0.49268)
 H022(0.855151) H023(0.708317) H024(0.663962) H02H(1.156156) H02I(1.158958)
 H02J(1.086248) H02A(0.451015) H02B(0.475371) H02C(0.580193) H028(0.627454)
 H029(0.784456) H02D(0.99975) H02E(1.037893) H02F(1.102739) H02G(1.102169)
 H02Q(0.549246) H02V(0.678539) H02K(0.513215) H02L(0.522056) H02M(0.636289)
 Fixed Z: H00C(0.261963) H00I(0.485055) H00M(0.256849) H00O(0.496234)
 H00P(0.497395) H00V(0.249658) H00X(0.363873) H00Y(0.25014) H00A(0.200782)
 H00B(0.196243) H01A(0.054269) H01B(0.050542) H011(0.393966) H012(0.501489)
 H013(0.499354) H014(0.25315) H015(0.384503) H016(0.247889) H01H(0.693415)
 H01I(0.696002) H018(0.354181) H019(0.496941) H01J(0.546364) H01K(0.549656)
 H01C(0.096919) H01D(0.112051) H01L(0.625793) H01M(0.623948) H01P(0.074838)
 H01Q(0.193881) H01R(0.675282) H01S(0.079607) H01T(0.555432) H01E(0.114638)
 H01F(0.109742) H01G(0.074701) H01V(0.063636) H01W(0.669653) H01N(0.639201)
 H01O(0.643462) H01U(0.678063) H01Y(0.575478) H01Z(0.182909) H020(0.169315)
 H022(0.555752) H023(0.683369) H024(0.569276) H02H(0.653259) H02I(0.65547)
 H02J(0.688725) H02A(0.170261) H02B(0.128984) H02C(0.161533) H028(0.075955)
 H029(0.193439) H02D(0.177864) H02E(0.066317) H02F(0.105388) H02G(0.098206)
 H02Q(0.576409) H02V(0.670839) H02K(0.574981) H02L(0.617476) H02M(0.588437)
;
_shelx_res_checksum              68007
_olex2_submission_special_instructions 'No special instructions were received'