Cobalt Complexes Containing Pendant Amines in the Second Coordination Sphere as Electrocatalysts for H2Production
Fang, Ming; Wiedner, Eric S.; Dougherty, William G.; Kassel, W. Scott; Liu, Tianbiao; DuBois, Daniel L.; Bullock, R. Morris; Organometallics 33 (2014) 5820–; doi:10.1021/om5004607

data_4083849
_publ_section_title
;
 Cobalt Complexes Containing Pendant Amines in the Second Coordination
 Sphere as Electrocatalysts for H2Production
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5820
_journal_paper_doi               10.1021/om5004607
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C35 H40 Co F5 N2 P2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C36 H41.5 Co F5 N2.5 P2'
_chemical_formula_weight         725.08
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                83.7820(10)
_cell_angle_beta                 75.9990(10)
_cell_angle_gamma                73.1910(10)
_cell_formula_units_Z            4
_cell_length_a                   14.1542(5)
_cell_length_b                   15.3241(5)
_cell_length_c                   16.4079(5)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.91
_cell_measurement_theta_min      2.21
_cell_volume                     3302.79(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68873
_diffrn_reflns_theta_full        33.18
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.9606
_exptl_absorpt_correction_T_min  0.8656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         25105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.3786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                16299
_reflns_number_total             25105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5004607_si_002.cif
_cod_data_source_block           pnl131_Co(I)CpC6F5
_cod_database_code               4083849
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.032) H2B(0.032) H2C(0.032) H3A(0.033) H3B(0.033) H3C(0.033)
 H4A(0.034) H4B(0.034) H4C(0.034) H5A(0.019) H5B(0.019) H6A(0.024) H7A(0.027)
 H8A(0.027) H9A(0.031) H10A(0.029) H12A(0.019) H12B(0.019) H14A(0.034)
 H14B(0.034) H14C(0.034) H15A(0.033) H15B(0.033) H15C(0.033) H16A(0.047)
 H16B(0.047) H16C(0.047) H17A(0.019) H17B(0.019) H18A(0.03) H19A(0.041)
 H20A(0.044) H21A(0.039) H22A(0.029) H24A(0.02) H24B(0.02) H26A(0.022)
 H27A(0.025) H28A(0.024) H29A(0.021) H37A(0.042) H37B(0.042) H37C(0.042)
 H38A(0.034) H38B(0.034) H38C(0.034) H39A(0.037) H39B(0.037) H39C(0.037)
 H40A(0.02) H40B(0.02) H41A(0.023) H42A(0.027) H43A(0.027) H44A(0.029)
 H45A(0.027) H47A(0.019) H47B(0.019) H49A(0.033) H49B(0.033) H49C(0.033)
 H50A(0.037) H50B(0.037) H50C(0.037) H51A(0.039) H51B(0.039) H51C(0.039)
 H52A(0.021) H52B(0.021) H53A(0.027) H54A(0.035) H55A(0.039) H56A(0.035)
 H57A(0.028) H59A(0.021) H59B(0.021) H61A(0.025) H62A(0.03) H63A(0.031)
 H64A(0.025) H71A(0.095) H71B(0.095) H71C(0.095)
 Fixed X: H2A(0.7533) H2B(0.659) H2C(0.772) H3A(0.8211) H3B(0.8816)
 H3C(0.8213) H4A(0.6315) H4B(0.6353) H4C(0.5711) H5A(0.5472) H5B(0.5699)
 H6A(0.6398) H7A(0.6438) H8A(0.6198) H9A(0.5939) H10A(0.5889) H12A(0.6067)
 H12B(0.5718) H14A(0.7229) H14B(0.6401) H14C(0.7046) H15A(0.9052) H15B(0.8845)
 H15C(0.9413) H16A(0.8259) H16B(0.8377) H16C(0.7277) H17A(0.708) H17B(0.7988)
 H18A(0.5546) H19A(0.4778) H20A(0.4871) H21A(0.568) H22A(0.6476) H24A(0.7607)
 H24B(0.6467) H26A(0.963) H27A(1.0225) H28A(0.9995) H29A(0.9267) H37A(0.3043)
 H37B(0.2035) H37C(0.312) H38A(0.2) H38B(0.192) H38C(0.1219) H39A(0.3843)
 H39B(0.4275) H39C(0.3755) H40A(0.0635) H40B(0.0955) H41A(0.1451) H42A(0.1492)
 H43A(0.1134) H44A(0.0729) H45A(0.0639) H47A(0.0727) H47B(0.051) H49A(0.2614)
 H49B(0.29) H49C(0.1738) H50A(0.1524) H50B(0.0833) H50C(0.1437) H51A(0.3376)
 H51B(0.3325) H51C(0.393) H52A(0.1686) H52B(0.2774) H53A(0.2039) H54A(0.1305)
 H55A(0.0053) H56A(-0.0496) H57A(0.0206) H59A(0.2899) H59B(0.1891) H61A(0.4519)
 H62A(0.5144) H63A(0.5059) H64A(0.4382) H71A(0.2815) H71B(0.2197) H71C(0.1641)
 Fixed Y: H2A(0.567) H2B(0.6236) H2C(0.6133) H3A(0.4031) H3B(0.438)
 H3C(0.3642) H4A(0.4651) H4B(0.4063) H4C(0.5111) H5A(0.5641) H5B(0.6291)
 H6A(0.795) H7A(0.9406) H8A(0.9904) H9A(0.8886) H10A(0.7426) H12A(0.6829)
 H12B(0.5947) H14A(0.5954) H14B(0.614) H14C(0.5119) H15A(0.5297) H15B(0.4559)
 H15C(0.5287) H16A(0.6912) H16B(0.6938) H16C(0.7252) H17A(0.4411) H17B(0.3979)
 H18A(0.4332) H19A(0.3281) H20A(0.191) H21A(0.1622) H22A(0.2656) H24A(0.3617)
 H24B(0.3957) H26A(0.6378) H27A(0.4608) H28A(0.4174) H29A(0.5668) H37A(0.5321)
 H37B(0.6146) H37C(0.6346) H38A(0.5023) H38B(0.5612) H38C(0.6016) H39A(0.4884)
 H39B(0.5737) H39C(0.5664) H40A(0.7771) H40B(0.7399) H41A(0.7582) H42A(0.7914)
 H43A(0.9422) H44A(1.0597) H45A(1.0289) H47A(0.9986) H47B(0.9316) H49A(1.1378)
 H49B(1.039) H49C(1.0955) H50A(1.1592) H50B(1.0981) H50C(1.0712) H51A(1.0968)
 H51B(1.003) H51C(1.0016) H52A(0.9371) H52B(0.8641) H53A(0.8537) H54A(0.8264)
 H55A(0.7492) H56A(0.7021) H57A(0.7313) H59A(0.7047) H59B(0.6746) H61A(0.6811)
 H62A(0.6779) H63A(0.8421) H64A(0.9489) H71A(0.2345) H71B(0.1827) H71C(0.2802)
 Fixed Z: H2A(0.6294) H2B(0.5905) H2C(0.5368) H3A(0.6084) H3B(0.5215)
 H3C(0.5216) H4A(0.6521) H4B(0.576) H4C(0.5806) H5A(0.4254) H5B(0.4839)
 H6A(0.2491) H7A(0.27) H8A(0.4044) H9A(0.5196) H10A(0.5004) H12A(0.2374)
 H12B(0.2788) H14A(0.0295) H14B(0.1161) H14C(0.0929) H15A(0.034) H15B(0.1081)
 H15C(0.1194) H16A(0.0555) H16B(0.1497) H16C(0.1289) H17A(0.1983) H17B(0.2452)
 H18A(0.214) H19A(0.1848) H20A(0.264) H21A(0.3749) H22A(0.4045) H24A(0.3955)
 H24B(0.4486) H26A(0.2124) H27A(0.2295) H28A(0.3876) H29A(0.4695) H37A(0.2124)
 H37B(0.2318) H37C(0.2097) H38A(0.1194) H38B(0.0335) H38C(0.1206) H39A(0.0663)
 H39B(0.0677) H39C(-0.0069) H40A(0.0914) H40B(0.1784) H41A(0.2755) H42A(0.4086)
 H43A(0.4469) H44A(0.3472) H45A(0.2151) H47A(0.1026) H47B(0.0456) H49A(0.049)
 H49B(0.0944) H49C(0.1037) H50A(-0.059) H50B(-0.0043) H50C(-0.098) H51A(-
 0.0984) H51B(-0.1292) H51C(-0.0581) H52A(-0.1107) H52B(-0.1236) H53A(-0.2332)
 H54A(-0.3376) H55A(-0.3042) H56A(-0.1653) H57A(-0.0596) H59A(-0.0775) H59B(-
 0.0356) H61A(0.1561) H62A(-0.0065) H63A(-0.0645) H64A(0.0619) H71A(0.3232)
 H71B(0.285) H71C(0.3248)
;