Variable coordination of carbazolyl-bis(tetrazole) ligands in lanthanide chemistry.
Gajecki, Leah; Berg, David J.; Hoenisch, Josh; Oliver, Allen G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15487–15496; doi:10.1039/c8dt02757a

data_7047760
_publ_section_title
;
 Variable coordination of carbazolyl-bis(tetrazole) ligands in lanthanide
 chemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15487
_journal_page_last               15496
_journal_paper_doi               10.1039/c8dt02757a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C59 H81 Er N18 O Si, 2.5(C7 H8)'
_chemical_formula_sum            'C76.5 H101 Er N18 O Si'
_chemical_formula_weight         1484.10
_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
_audit_creation_date             2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.643(3)
_cell_angle_beta                 88.231(3)
_cell_angle_gamma                88.254(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0938(7)
_cell_length_b                   15.8303(8)
_cell_length_c                   18.8202(9)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.176
_cell_volume                     3865.7(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       \f
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74280
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         1.799
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.9117
_exptl_absorpt_correction_T_min  0.7952
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.300
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         19078
_refine_ls_number_restraints     761
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+6.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15956
_reflns_number_total             19078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02757a2.cif
_cod_data_source_block           Compound_3a
_cod_depositor_comments
'Adding full bibliography for 7047755--7047762.cif.'
_cod_original_formula_sum        'C76.50 H101 Er N18 O Si'
_cod_database_code               7047760
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Others
 Fixed Sof: C7'(0.5) C8'(0.5) H8'A(0.5) H8'B(0.5) H8'C(0.5) C9'(0.5) H9'A(0.5)
 H9'B(0.5) H9'C(0.5) C10'(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C12(0.5) H12(0.5)
 C12'(0.5) H12'(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C13'(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14'(0.5) H14D(0.5)
 H14E(0.5) H14F(0.5) C200(0.5) C201(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C202(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C203(0.5) H20G(0.5) H20H(0.5)
 H20I(0.5) C208(0.5) H208(0.5) C209(0.5) H20S(0.5) H20T(0.5) H20U(0.5)
 C210(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C211(0.5) H211(0.5) C212(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C213(0.5) H21G(0.5) H21H(0.5) H21I(0.5)
 C122(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C123(0.5) C124(0.5) H124(0.5)
 C125(0.5) H125(0.5) C126(0.5) H126(0.5) C127(0.5) H127(0.5) C128(0.5)
 H128(0.5) C129(0.15) H12D(0.15) H12E(0.15) H12F(0.15) C130(0.15) C131(0.15)
 H131(0.15) C132(0.15) H132(0.15) C133(0.15) H133(0.15) C134(0.15) H134(0.15)
 C142(0.15) H142(0.15) C100(0.7) H10G(0.7) H10H(0.7) H10I(0.7) C101(0.7)
 C102(0.7) H102(0.7) C103(0.7) H103(0.7) C104(0.7) H104(0.7) C105(0.7)
 H105(0.7) C106(0.7) H106(0.7) C107(0.5) H10J(0.5) H10K(0.5) H10L(0.5)
 C108(0.5) C109(0.5) H109(0.5) C110(0.5) H110(0.5) C111(0.5) H111(0.5)
 C112(0.5) H112(0.5) C113(0.5) H113(0.5) C115(0.15) H11A(0.15) H11B(0.15)
 H11C(0.15) C116(0.15) C121(0.15) H121(0.15) C120(0.15) H120(0.15) C119(0.15)
 H119(0.15) C118(0.15) H118(0.15) C117(0.15) H117(0.15) C07(0.5) H07A(0.5)
 H07B(0.5) H07C(0.5) C01(0.5) C02(0.5) H02(0.5) C03(0.5) H03(0.5) C04(0.5)
 H04(0.5) C05(0.5) H05(0.5) C06(0.5) H06(0.5)
 Fixed Uiso: H3(0.041) H3'(0.066) H5(0.039) H5'(0.065) H8A(0.085) H8B(0.085)
 H8C(0.085) H8'A(0.059) H8'B(0.059) H8'C(0.059) H9A(0.086) H9B(0.086)
 H9C(0.086) H9'A(0.13) H9'B(0.13) H9'C(0.13) H10A(0.094) H10B(0.094)
 H10C(0.094) H10D(0.085) H10E(0.085) H10F(0.085) H12(0.035) H12'(0.054)
 H13A(0.048) H13B(0.048) H13C(0.048) H13D(0.138) H13E(0.138) H13F(0.138)
 H14A(0.053) H14B(0.053) H14C(0.053) H14D(0.135) H14E(0.135) H14F(0.135)
 H16(0.047) H17'(0.045) H18(0.037) H19'(0.051) H22A(0.15) H22B(0.15) H22C(0.15)
 H22D(0.116) H22E(0.116) H22F(0.116) H23A(0.083) H23B(0.083) H23C(0.083)
 H23D(0.127) H23E(0.127) H23F(0.127) H24A(0.093) H24B(0.093) H24C(0.093)
 H24D(0.134) H24E(0.134) H24F(0.134) H26(0.044) H26'(0.061) H27A(0.054)
 H27B(0.054) H27C(0.054) H27D(0.152) H27E(0.152) H27F(0.152) H28A(0.097)
 H28B(0.097) H28C(0.097) H28D(0.092) H28E(0.092) H28F(0.092) H29A(0.078)
 H29B(0.078) H29C(0.078) H30A(0.069) H30B(0.069) H30C(0.069) H31A(0.091)
 H31B(0.091) H31C(0.091) H20A(0.1) H20B(0.1) H20C(0.1) H20D(0.092) H20E(0.092)
 H20F(0.092) H20G(0.093) H20H(0.093) H20I(0.093) H20J(0.091) H20K(0.091)
 H20L(0.091) H20M(0.08) H20N(0.08) H20O(0.08) H20P(0.079) H20Q(0.079)
 H20R(0.079) H208(0.038) H20S(0.078) H20T(0.078) H20U(0.078) H21A(0.076)
 H21B(0.076) H21C(0.076) H211(0.042) H21D(0.06) H21E(0.06) H21F(0.06)
 H21G(0.106) H21H(0.106) H21I(0.106) H12A(0.082) H12B(0.082) H12C(0.082)
 H124(0.051) H125(0.053) H126(0.06) H127(0.055) H128(0.047) H12D(0.096)
 H12E(0.096) H12F(0.096) H131(0.072) H132(0.07) H133(0.076) H134(0.066)
 H142(0.066) H10G(0.212) H10H(0.212) H10I(0.212) H102(0.066) H103(0.063)
 H104(0.069) H105(0.074) H106(0.072) H10J(0.094) H10K(0.094) H10L(0.094)
 H109(0.041) H110(0.045) H111(0.044) H112(0.045) H113(0.042) H11A(0.072)
 H11B(0.072) H11C(0.072) H121(0.072) H120(0.077) H119(0.066) H118(0.058)
 H117(0.077) H07A(0.204) H07B(0.204) H07C(0.204) H02(0.079) H03(0.075)
 H04(0.07) H05(0.055) H06(0.071)
 Fixed X: H3(0.603005) H3'(0.127003) H5(0.540838) H5'(-0.063287) H8A(0.750057)
 H8B(0.758074) H8C(0.657815) H8'A(0.108942) H8'B(0.072871) H8'C(0.15569)
 H9A(0.719455) H9B(0.797782) H9C(0.784069) H9'A(0.030984) H9'B(-0.036279) H9'C(-
 0.086325) H10A(0.557273) H10B(0.661118) H10C(0.579451) H10D(-0.144986) H10E(-
 0.108289) H10F(-0.072452) H12(0.46416) H12'(0.477917) H13A(0.437221)
 H13B(0.528785) H13C(0.553141) H13D(0.382655) H13E(0.426981) H13F(0.310192)
 H14A(0.667622) H14B(0.644146) H14C(0.618668) H14D(0.350045) H14E(0.467831)
 H14F(0.436705) H16(0.407704) H17'(-0.000327) H18(0.217148) H19'(-0.106497)
 H22A(0.389954) H22B(0.284841) H22C(0.300802) H22D(-0.062778) H22E(-0.139481)
 H22F(-0.034241) H23A(0.279278) H23B(0.288915) H23C(0.384013) H23D(-0.138251)
 H23E(-0.237086) H23F(-0.232352) H24A(0.128712) H24B(0.13403) H24C(0.123854)
 H24D(-0.262119) H24E(-0.279434) H24F(-0.198582) H26(0.06802) H26'(0.188156)
 H27A(-0.00203) H27B(0.018628) H27C(0.095109) H27D(0.394026) H27E(0.350135)
 H27F(0.31306) H28A(0.245385) H28B(0.16755) H28C(0.235891) H28D(0.214421)
 H28E(0.29519) H28F(0.330356) H29A(-0.054181) H29B(-0.096518) H29C(0.019265)
 H30A(-0.090466) H30B(-0.16632) H30C(-0.12678) H31A(0.107532) H31B(-0.009212)
 H31C(0.058801) H20A(0.067789) H20B(-0.044707) H20C(-0.013333) H20D(-0.174301)
 H20E(-0.190596) H20F(-0.186811) H20G(-0.048539) H20H(-0.048737) H20I(0.055244)
 H20J(0.148975) H20K(0.209262) H20L(0.229462) H20M(0.410675) H20N(0.391122)
 H20O(0.455039) H20P(0.336395) H20Q(0.269572) H20R(0.216281) H208(0.549789)
 H20S(0.389167) H20T(0.469584) H20U(0.428535) H21A(0.614949) H21B(0.656054)
 H21C(0.681046) H211(0.413703) H21D(0.287487) H21E(0.360188) H21F(0.26464)
 H21G(0.513536) H21H(0.51125) H21I(0.442803) H12A(0.543406) H12B(0.548933)
 H12C(0.597164) H124(0.486231) H125(0.330847) H126(0.189762) H127(0.205491)
 H128(0.361049) H12D(0.587315) H12E(0.655547) H12F(0.59211) H131(0.428876)
 H132(0.290059) H133(0.280908) H134(0.410576) H142(0.549394) H10G(0.257871)
 H10H(0.272636) H10I(0.321565) H102(0.441761) H103(0.59375) H104(0.646405)
 H105(0.545355) H106(0.393454) H10J(0.167562) H10K(0.241152) H10L(0.208725)
 H109(0.242896) H110(0.382113) H111(0.542874) H112(0.565083) H113(0.423197)
 H11A(0.480348) H11B(0.592264) H11C(0.57107) H121(0.369263) H120(0.334279)
 H119(0.459063) H118(0.618833) H117(0.653819) H07A(0.085117) H07B(-0.001556)
 H07C(0.110033) H02(-0.021483) H03(-0.075851) H04(-0.061114) H05(0.00799)
 H06(0.062358)
 Fixed Y: H3(0.242579) H3'(0.734488) H5(0.039439) H5'(0.673359) H8A(0.171434)
 H8B(0.084315) H8C(0.14446) H8'A(0.856971) H8'B(0.93427) H8'C(0.865272)
 H9A(0.015478) H9B(0.009137) H9C(0.09648) H9'A(0.828006) H9'B(0.906458)
 H9'C(0.815331) H10A(0.016087) H10B(-0.038982) H10C(-0.034632) H10D(0.802212)
 H10E(0.896541) H10F(0.81891) H12(0.592248) H12'(0.604078) H13A(0.499352)
 H13B(0.561208) H13C(0.464767) H13D(0.529024) H13E(0.608753) H13F(0.610336)
 H14A(0.517223) H14B(0.613783) H14C(0.58359) H14D(0.750864) H14E(0.743167)
 H14F(0.741033) H16(0.004203) H17'(0.28982) H18(0.142146) H19'(0.532175) H22A(-
 0.103996) H22B(-0.150839) H22C(-0.099836) H22D(0.284487) H22E(0.327803)
 H22F(0.372196) H23A(0.03975) H23B(-0.061833) H23C(-0.0087) H23D(0.507978)
 H23E(0.456711) H23F(0.500733) H24A(-0.026394) H24B(-0.077866) H24C(0.023938)
 H24D(0.365133) H24E(0.32181) H24F(0.280428) H26(0.39263) H26'(0.049649)
 H27A(0.492103) H27B(0.537952) H27C(0.550908) H27D(0.104276) H27E(0.025974)
 H27F(0.121353) H28A(0.494086) H28B(0.481051) H28C(0.402224) H28D(0.018791)
 H28E(-0.034995) H28F(0.04811) H29A(0.303264) H29B(0.209256) H29C(0.222054)
 H30A(0.268374) H30B(0.241091) H30C(0.336573) H31A(0.117141) H31B(0.094226)
 H31C(0.129735) H20A(0.870276) H20B(0.911622) H20C(0.82727) H20D(0.763285)
 H20E(0.853088) H20F(0.766843) H20G(0.804099) H20H(0.897733) H20I(0.841894)
 H20J(0.00393) H20K(-0.059638) H20L(0.040389) H20M(0.005199) H20N(-0.094369)
 H20O(-0.044703) H20P(-0.107991) H20Q(-0.147892) H20R(-0.086749) H208(0.593175)
 H20S(0.593716) H20T(0.621285) H20U(0.526186) H21A(0.473828) H21B(0.568652)
 H21C(0.500902) H211(0.712187) H21D(0.649278) H21E(0.728944) H21F(0.734785)
 H21G(0.590999) H21H(0.636986) H21I(0.555651) H12A(0.136263) H12B(0.196411)
 H12C(0.226408) H124(0.28597) H125(0.353413) H126(0.345949) H127(0.269802)
 H128(0.202358) H12D(0.690366) H12E(0.751005) H12F(0.789858) H131(0.654392)
 H132(0.682812) H133(0.81016) H134(0.909087) H142(0.880668) H10G(0.721329)
 H10H(0.816829) H10I(0.738484) H102(0.883723) H103(0.890324) H104(0.775669)
 H105(0.654549) H106(0.648112) H10J(0.283015) H10K(0.260955) H10L(0.187234)
 H109(0.328055) H110(0.349595) H111(0.300508) H112(0.228953) H113(0.209741)
 H11A(0.604887) H11B(0.599707) H11C(0.657093) H121(0.677414) H120(0.784752)
 H119(0.883442) H118(0.874794) H117(0.767456) H07A(-0.169641) H07B(-0.141579)
 H07C(-0.102841) H02(0.019012) H03(0.138003) H04(0.136687) H05(0.016379) H06(-
 0.102613)
 Fixed Z: H3(0.820091) H3'(0.632744) H5(0.719539) H5'(0.802241) H8A(0.854964)
 H8B(0.908214) H8C(0.910174) H8'A(0.77108) H8'B(0.713232) H8'C(0.690992)
 H9A(0.736688) H9B(0.80089) H9C(0.748558) H9'A(0.587499) H9'B(0.610879)
 H9'C(0.611825) H10A(0.895435) H10B(0.890037) H10C(0.828051) H10D(0.73433)
 H10E(0.740107) H10F(0.797718) H12(0.836832) H12'(0.487021) H13A(0.942729)
 H13B(0.952478) H13C(0.939017) H13D(0.422121) H13E(0.370783) H13F(0.398393)
 H14A(0.828562) H14B(0.842032) H14C(0.766721) H14D(0.453161) H14E(0.428911)
 H14F(0.512009) H16(0.614903) H17'(0.935767) H18(0.477248) H19'(0.895665)
 H22A(0.546836) H22B(0.539724) H22C(0.606496) H22D(1.040146) H22E(1.093545)
 H22F(1.067577) H23A(0.408556) H23B(0.413377) H23C(0.432737) H23D(1.023793)
 H23E(1.054253) H23F(0.972828) H24A(0.565532) H24B(0.497601) H24C(0.486298)
 H24D(0.922601) H24E(1.003509) H24F(0.951626) H26(0.3601) H26'(0.917481)
 H27A(0.432176) H27B(0.352418) H27C(0.414605) H27D(0.911062) H27E(0.964321)
 H27F(0.973415) H28A(0.338958) H28B(0.277604) H28C(0.313176) H28D(0.801379)
 H28E(0.852315) H28F(0.800948) H29A(0.54606) H29B(0.566592) H29C(0.538481)
 H30A(0.76815) H30B(0.710542) H30C(0.702992) H31A(0.670563) H31B(0.689368)
 H31C(0.747654) H20A(0.654246) H20B(0.644122) H20C(0.609114) H20D(0.675107)
 H20E(0.704967) H20F(0.759535) H20G(0.828453) H20H(0.784759) H20I(0.792051)
 H20J(0.466463) H20K(0.419291) H20L(0.405294) H20M(0.416887) H20N(0.437312)
 H20O(0.489239) H20P(0.585105) H20Q(0.528544) H20R(0.58104) H208(0.785118)
 H20S(0.843819) H20T(0.89833) H20U(0.908471) H21A(0.901867) H21B(0.884837)
 H21C(0.830061) H211(0.507051) H21D(0.404706) H21E(0.385727) H21F(0.440153)
 H21G(0.507387) H21H(0.426591) H21I(0.450552) H12A(1.056737) H12B(1.118607)
 H12C(1.040621) H124(0.943012) H125(0.908698) H126(0.989309) H127(1.104282)
 H128(1.138278) H12D(0.629038) H12E(0.668915) H12F(0.600439) H131(0.685152)
 H132(0.760575) H133(0.811622) H134(0.787248) H142(0.711826) H10G(0.761502)
 H10H(0.778) H10I(0.829209) H102(0.752834) H103(0.684095) H104(0.622576)
 H105(0.63055) H106(0.699451) H10J(1.083386) H10K(1.149935) H10L(1.105038)
 H109(0.96701) H110(0.891106) H111(0.92664) H112(1.043019) H113(1.120465)
 H11A(0.612252) H11B(0.644655) H11C(0.569941) H121(0.685685) H120(0.758337)
 H119(0.772759) H118(0.71453) H117(0.641878) H07A(1.004297) H07B(0.947231)
 H07C(0.935139) H02(0.919127) H03(0.973637) H04(1.09737) H05(1.166595)
 H06(1.112086)
;
_shelx_res_checksum              12015
_olex2_submission_special_instructions 'No special instructions were received'