Controlling proton movement: electrocatalytic oxidation of hydrogen by a nickel(ii) complex containing proton relays in the second and outer coordination spheres.
Das, Parthapratim; Ho, Ming-Hsun; O'Hagan, Molly; Shaw, Wendy J.; Morris Bullock, R.; Raugei, Simone; Helm, Monte L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2744–2754; doi:10.1039/c3dt53074d

data_7028418
_publ_section_title
;
 Controlling proton movement: electrocatalytic oxidation of hydrogen by a
 nickel(ii) complex containing proton relays in the second and outer
 coordination spheres.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2744
_journal_page_last               2754
_journal_paper_doi               10.1039/c3dt53074d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C44 H88 N4 Ni O4 P4, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C46 H91 B2 F8 N5 Ni O4 P4'
_chemical_formula_weight         1134.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-10-24
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_cell_angle_alpha                68.287(3)
_cell_angle_beta                 89.983(3)
_cell_angle_gamma                90.010(3)
_cell_formula_units_Z            4
_cell_length_a                   10.6652(11)
_cell_length_b                   20.820(2)
_cell_length_c                   27.135(3)
_cell_measurement_reflns_used    7105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.26
_cell_volume                     5597.8(10)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.1282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.233
_diffrn_reflns_theta_min         0.808
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1282
_refine_ls_number_reflns         24841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0393P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15639
_reflns_number_total             24841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53074d.txt
_cod_data_source_block           p1bar
_cod_original_cell_volume        5597.8(9)
_cod_database_code               7028418
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.022) H1B(0.022) H2A(0.023) H2B(0.023) H3A(0.021) H3B(0.021)
 H4A(0.023) H4B(0.023) H5(0.02) H6A(0.027) H6B(0.027) H7A(0.031) H7B(0.031)
 H8A(0.036) H8B(0.036) H9A(0.03) H9B(0.03) H10A(0.022) H10B(0.022) H11A(0.024)
 H11B(0.024) H12A(0.029) H12B(0.029) H13A(0.056) H13B(0.056) H13C(0.056)
 H14(0.023) H15A(0.025) H15B(0.025) H16A(0.033) H16B(0.033) H17A(0.041)
 H17B(0.041) H18A(0.037) H18B(0.037) H19A(0.027) H19B(0.027) H20A(0.024)
 H20B(0.024) H21A(0.036) H21B(0.036) H22A(0.066) H22B(0.066) H22C(0.066)
 H23A(0.026) H23B(0.026) H24A(0.027) H24B(0.027) H25A(0.025) H25B(0.025)
 H26A(0.023) H26B(0.023) H27(0.021) H28A(0.025) H28B(0.025) H29A(0.03)
 H29B(0.03) H30A(0.03) H30B(0.03) H31A(0.029) H31B(0.029) H32A(0.027)
 H32B(0.027) H33A(0.034) H33B(0.034) H34A(0.042) H34B(0.042) H35A(0.07)
 H35B(0.07) H35C(0.07) H36(0.024) H37A(0.031) H37B(0.031) H38A(0.038)
 H38B(0.038) H39A(0.038) H39B(0.038) H40A(0.038) H40B(0.038) H41A(0.028)
 H41B(0.028) H42A(0.02) H42B(0.02) H43A(0.028) H43B(0.028) H44A(0.057)
 H44B(0.057) H44C(0.057) H45A(0.021) H45B(0.021) H46A(0.02) H46B(0.02)
 H47A(0.027) H47B(0.027) H48A(0.023) H48B(0.023) H49(0.023) H50A(0.028)
 H50B(0.028) H51A(0.035) H51B(0.035) H52A(0.037) H52B(0.037) H53A(0.033)
 H53B(0.033) H54A(0.026) H54B(0.026) H55A(0.027) H55B(0.027) H56A(0.027)
 H56B(0.027) H57A(0.066) H57B(0.066) H57C(0.066) H58(0.024) H59A(0.028)
 H59B(0.028) H60A(0.04) H60B(0.04) H61A(0.054) H61B(0.054) H62A(0.054)
 H62B(0.054) H63A(0.029) H63B(0.029) H64A(0.033) H64B(0.033) H65A(0.029)
 H65B(0.029) H66A(0.054) H66B(0.054) H66C(0.054) H67A(0.031) H67B(0.031)
 H68A(0.029) H68B(0.029) H69A(0.026) H69B(0.026) H70A(0.023) H70B(0.023)
 H71(0.025) H72A(0.028) H72B(0.028) H73A(0.033) H73B(0.033) H74A(0.039)
 H74B(0.039) H75A(0.037) H75B(0.037) H76A(0.029) H76B(0.029) H77A(0.048)
 H77B(0.048) H77C(0.048) H77D(0.048) H78A(0.03) H78B(0.03) H79A(0.106)
 H79B(0.106) H79C(0.106) H80(0.025) H81A(0.029) H81B(0.029) H82A(0.034)
 H82B(0.034) H83A(0.043) H83B(0.043) H84A(0.042) H84B(0.042) H85A(0.037)
 H85B(0.037) H86A(0.025) H86B(0.025) H87A(0.031) H87B(0.031) H88A(0.052)
 H88B(0.052) H88C(0.052) H90A(0.107) H90B(0.107) H90C(0.107) H92A(0.121)
 H92B(0.121) H92C(0.121) H78C(0.029) H78D(0.029)
 Fixed X: H1A(0.5932) H1B(0.6149) H2A(0.569) H2B(0.5339) H3A(0.4814)
 H3B(0.3762) H4A(0.2852) H4B(0.4291) H5(0.4187) H6A(0.52) H6B(0.6014)
 H7A(0.6018) H7B(0.55) H8A(0.3976) H8B(0.4163) H9A(0.308) H9B(0.222)
 H10A(0.2759) H10B(0.2159) H11A(0.5258) H11B(0.4303) H12A(0.5688) H12B(0.6836)
 H13A(0.6107) H13B(0.7136) H13C(0.587) H14(0.2187) H15A(0.2305) H15B(0.3729)
 H16A(0.2408) H16B(0.16) H17A(0.4161) H17B(0.2993) H18A(0.4106) H18B(0.268)
 H19A(0.4791) H19B(0.3998) H20A(0.1278) H20B(0.167) H21A(0.0339) H21B(0.1337)
 H22A(0.1382) H22B(0.04) H22C(0.17) H23A(0.0592) H23B(0.2049) H24A(0.0458)
 H24B(-0.0271) H25A(-0.1264) H25B(-0.1044) H26A(0.0358) H26B(-0.0409)
 H27(0.2623) H28A(0.4362) H28B(0.3753) H29A(0.5239) H29B(0.454) H30A(0.3966)
 H30B(0.3534) H31A(0.1742) H31B(0.2308) H32A(0.1556) H32B(0.0823) H33A(0.218)
 H33B(0.0987) H34A(0.3412) H34B(0.2219) H35A(0.4302) H35B(0.4388) H35C(0.3336)
 H36(0.0455) H37A(-0.1973) H37B(-0.1337) H38A(-0.2751) H38B(-0.1352) H39A(-
 0.2242) H39B(-0.2573) H40A(-0.008) H40B(-0.0757) H41A(-0.0697) H41B(0.0699)
 H42A(-0.153) H42B(-0.1762) H43A(-0.1309) H43B(0.0073) H44A(-0.1555) H44B(-
 0.0925) H44C(-0.1901) H45A(-0.1176) H45B(-0.0948) H46A(-0.0348) H46B(-0.0722)
 H47A(0.0583) H47B(0.2015) H48A(0.12) H48B(0.0104) H49(0.0742) H50A(-0.1066)
 H50B(-0.0207) H51A(-0.109) H51B(-0.0542) H52A(0.095) H52B(0.0756) H53A(0.1869)
 H53B(0.2741) H54A(0.279) H54B(0.2194) H55A(0.0689) H55B(-0.0311) H56A(-0.1818)
 H56B(-0.0684) H57A(-0.1031) H57B(-0.1138) H57C(-0.2187) H58(0.2784)
 H59A(0.2689) H59B(0.1272) H60A(0.2641) H60B(0.3415) H61A(0.084) H61B(0.1989)
 H62A(0.2323) H62B(0.0906) H63A(0.0179) H63B(0.097) H64A(0.3279) H64B(0.36)
 H65A(0.3439) H65B(0.4561) H66A(0.4625) H66B(0.3612) H66C(0.3382) H67A(0.2918)
 H67B(0.439) H68A(0.5365) H68B(0.4727) H69A(0.6005) H69B(0.6287) H70A(0.5416)
 H70B(0.4643) H71(0.2356) H72A(0.0668) H72B(0.1297) H73A(-0.0241) H73B(0.0477)
 H74A(0.1446) H74B(0.1018) H75A(0.2684) H75B(0.324) H76A(0.4167) H76B(0.3442)
 H77A(0.3156) H77B(0.4234) H77C(0.3825) H77D(0.3839) H78A(0.1771) H78B(0.2887)
 H79A(0.037) H79B(0.1007) H79C(0.112) H80(0.4593) H81A(0.5639) H81B(0.4249)
 H82A(0.5636) H82B(0.5054) H83A(0.7182) H83B(0.75) H84A(0.6453) H84B(0.7832)
 H85A(0.6993) H85B(0.6441) H86A(0.6749) H86B(0.6468) H87A(0.4822) H87B(0.6202)
 H88A(0.6632) H88B(0.6847) H88C(0.5931) H90A(0.9304) H90B(0.9899) H90C(1.0782)
 H92A(0.5747) H92B(0.4918) H92C(0.4272) H78C(0.1756) H78D(0.1633)
 Fixed Y: H1A(0.0106) H1B(-0.0622) H2A(-0.0725) H2B(-0.0051) H3A(-0.1621) H3B(-
 0.1694) H4A(-0.1725) H4B(-0.1705) H5(0.0048) H6A(-0.1328) H6B(-0.0636) H7A(-
 0.1057) H7B(-0.0282) H8A(-0.1495) H8B(-0.0919) H9A(-0.0112) H9B(-0.0782) H10A(-
 0.1202) H10B(-0.0446) H11A(0.1034) H11B(0.0838) H12A(0.1799) H12B(0.1264)
 H13A(0.1403) H13B(0.1601) H13C(0.2041) H14(-0.0687) H15A(0.0529) H15B(0.0523)
 H16A(0.0839) H16B(0.0147) H17A(0.0194) H17B(-0.0017) H18A(-0.1018) H18B(-
 0.1035) H19A(-0.0642) H19B(-0.1341) H20A(-0.1635) H20B(-0.1218) H21A(-0.2156)
 H21B(-0.2685) H22A(-0.3235) H22B(-0.2664) H22C(-0.2765) H23A(0.1734)
 H23B(0.1924) H24A(0.1179) H24B(0.1305) H25A(0.0288) H25B(-0.0505) H26A(0.0353)
 H26B(0.078) H27(0.0676) H28A(0.1064) H28B(0.1821) H29A(0.1791) H29B(0.1144)
 H30A(0.2146) H30B(0.2518) H31A(0.212) H31B(0.1355) H32A(0.2028) H32B(0.1397)
 H33A(0.2496) H33B(0.236) H34A(0.1833) H34B(0.1789) H35A(0.343) H35B(0.2833)
 H35C(0.3419) H36(-0.0037) H37A(-0.0021) H37B(0.0639) H38A(0.0086) H38B(0.0074)
 H39A(-0.102) H39B(-0.106) H40A(-0.1078) H40B(-0.1722) H41A(-0.1151) H41B(-
 0.1175) H42A(-0.0922) H42B(-0.0227) H43A(-0.1219) H43B(-0.1221) H44A(0.0244)
 H44B(0.0159) H44C(-0.0407) H45A(0.4245) H45B(0.4974) H46A(0.4796) H46B(0.413)
 H47A(0.3151) H47B(0.3094) H48A(0.3175) H48B(0.3244) H49(0.4935) H50A(0.421)
 H50B(0.3542) H51A(0.3885) H51B(0.465) H52A(0.3433) H52B(0.4044) H53A(0.4828)
 H53B(0.417) H54A(0.4449) H54B(0.3695) H55A(0.5706) H55B(0.5905) H56A(0.6102)
 H56B(0.6645) H57A(0.6241) H57B(0.6862) H57C(0.627) H58(0.4152) H59A(0.5356)
 H59B(0.5363) H60A(0.5673) H60B(0.4969) H61A(0.5042) H61B(0.4832) H62A(0.3815)
 H62B(0.3828) H63A(0.4199) H63B(0.35) H64A(0.3612) H64B(0.316) H65A(0.2144)
 H65B(0.2643) H66A(0.2314) H66B(0.1722) H66C(0.2264) H67A(0.6748) H67B(0.6589)
 H68A(0.6064) H68B(0.5934) H69A(0.4261) H69B(0.5058) H70A(0.5631) H70B(0.5246)
 H71(0.5562) H72A(0.5946) H72B(0.6698) H73A(0.6667) H73B(0.6036) H74A(0.7412)
 H74B(0.7061) H75A(0.6278) H75B(0.7044) H76A(0.6281) H76B(0.6902) H77A(0.7305)
 H77B(0.705) H77C(0.7307) H77D(0.6873) H78A(0.6614) H78B(0.6655) H79A(0.766)
 H79B(0.8359) H79C(0.8146) H80(0.4733) H81A(0.3591) H81B(0.3602) H82A(0.3022)
 H82B(0.3692) H83A(0.3659) H83B(0.3598) H84A(0.4785) H84B(0.474) H85A(0.4671)
 H85B(0.5347) H86A(0.4626) H86B(0.3901) H87A(0.371) H87B(0.3697) H88A(0.5157)
 H88B(0.4544) H88C(0.5171) H90A(0.2159) H90B(0.14) H90C(0.2059) H92A(0.7205)
 H92B(0.755) H92C(0.7057) H78C(0.732) H78D(0.6696)
 Fixed Z: H1A(0.8036) H1B(0.7979) H2A(0.7145) H2B(0.6647) H3A(0.8279)
 H3B(0.8713) H4A(0.7308) H4B(0.7465) H5(0.8766) H6A(0.9177) H6B(0.8923)
 H7A(0.9881) H7B(0.9626) H8A(1.0068) H8B(1.0321) H9A(0.9617) H9B(0.989)
 H10A(0.9212) H10B(0.8948) H11A(0.7378) H11B(0.7002) H12A(0.6527) H12B(0.668)
 H13A(0.5405) H13B(0.5754) H13C(0.5587) H14(0.6464) H15A(0.6221) H15B(0.6034)
 H16A(0.5288) H16B(0.5555) H17A(0.5219) H17B(0.494) H18A(0.5497) H18B(0.5688)
 H19A(0.6174) H19B(0.6439) H20A(0.7839) H20B(0.8205) H21A(0.8668) H21B(0.859)
 H22A(0.9553) H22B(0.9574) H22C(0.9889) H23A(0.738) H23B(0.7372) H24A(0.6378)
 H24B(0.685) H25A(0.7597) H25B(0.7679) H26A(0.8645) H26B(0.8118) H27(0.8717)
 H28A(0.8123) H28B(0.7883) H29A(0.8534) H29B(0.8963) H30A(0.9113) H30B(0.8508)
 H31A(0.9034) H31B(0.9282) H32A(0.8195) H32B(0.8627) H33A(0.6549) H33B(0.6242)
 H34A(0.6176) H34B(0.5832) H35A(0.5453) H35B(0.6029) H35C(0.5908) H36(0.6375)
 H37A(0.6828) H37B(0.6385) H38A(0.5981) H38B(0.5769) H39A(0.5979) H39B(0.6565)
 H40A(0.6167) H40B(0.661) H41A(0.7222) H41B(0.7009) H42A(0.8501) H42B(0.8609)
 H43A(0.9385) H43B(0.916) H44A(0.9201) H44B(0.9756) H44C(0.9723) H45A(0.2993)
 H45B(0.3047) H46A(0.1659) H46B(0.216) H47A(0.2494) H47B(0.2342) H48A(0.3742)
 H48B(0.3327) H49(0.3764) H50A(0.3944) H50B(0.4224) H51A(0.4884) H51B(0.4601)
 H52A(0.5109) H52B(0.5327) H53A(0.4588) H53B(0.4878) H54A(0.3943) H54B(0.4231)
 H55A(0.2021) H55B(0.2381) H56A(0.1676) H56B(0.1532) H57A(0.0412) H57B(0.0624)
 H57C(0.0779) H58(0.1482) H59A(0.1256) H59B(0.1058) H60A(0.0308) H60B(0.0579)
 H61A(0.0245) H61B(-0.0046) H62A(0.0705) H62B(0.0505) H63A(0.1189) H63B(0.1455)
 H64A(0.3199) H64B(0.2851) H65A(0.3631) H65B(0.3656) H66A(0.4544) H66B(0.4604)
 H66C(0.4887) H67A(0.2302) H67B(0.2352) H68A(0.1891) H68B(0.1402) H69A(0.2741)
 H69B(0.2625) H70A(0.3096) H70B(0.363) H71(0.3693) H72A(0.3082) H72B(0.2846)
 H73A(0.349) H73B(0.3927) H74A(0.344) H74B(0.4047) H75A(0.4235) H75B(0.3964)
 H76A(0.3585) H76B(0.314) H77A(0.1466) H77B(0.1171) H77C(0.1421) H77D(0.1042)
 H78A(0.1154) H78B(0.0743) H79A(0.0702) H79B(0.031) H79C(0.0939) H80(0.1409)
 H81A(0.2261) H81B(0.2034) H82A(0.1653) H82B(0.1202) H83A(0.1048) H83B(0.164)
 H84A(0.083) H84B(0.1074) H85A(0.1899) H85B(0.1443) H86A(0.3625) H86B(0.3569)
 H87A(0.4219) H87B(0.4449) H88A(0.42) H88B(0.4761) H88C(0.4717) H90A(0.43)
 H90B(0.4505) H90C(0.44) H92A(-0.0678) H92B(-0.0351) H92C(-0.0611) H78C(0.1449)
 H78D(0.1236)
;
_shelx_hkl_checksum              57549
_shelx_res_checksum              54494
_shelxl_version_number           2013-2